CN216192002U - Continuous production device for oxamide - Google Patents
Continuous production device for oxamide Download PDFInfo
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- CN216192002U CN216192002U CN202122766298.5U CN202122766298U CN216192002U CN 216192002 U CN216192002 U CN 216192002U CN 202122766298 U CN202122766298 U CN 202122766298U CN 216192002 U CN216192002 U CN 216192002U
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- oxamide
- liquid phase
- dimethyl oxalate
- methanol
- tank
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- YIKSCQDJHCMVMK-UHFFFAOYSA-N Oxamide Chemical compound NC(=O)C(N)=O YIKSCQDJHCMVMK-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000010924 continuous production Methods 0.000 title claims abstract description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 196
- LOMVENUNSWAXEN-UHFFFAOYSA-N Methyl oxalate Chemical compound COC(=O)C(=O)OC LOMVENUNSWAXEN-UHFFFAOYSA-N 0.000 claims abstract description 74
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000007791 liquid phase Substances 0.000 claims abstract description 61
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- 238000003860 storage Methods 0.000 claims abstract description 34
- 238000011010 flushing procedure Methods 0.000 claims abstract description 30
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 239000012071 phase Substances 0.000 claims abstract description 21
- 238000010992 reflux Methods 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims description 53
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 29
- 238000011084 recovery Methods 0.000 claims description 29
- 239000000706 filtrate Substances 0.000 claims description 28
- 238000000926 separation method Methods 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 22
- 238000001914 filtration Methods 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000007790 solid phase Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 abstract description 12
- 239000000463 material Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000005915 ammonolysis reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 125000003917 carbamoyl group Chemical group [H]N([H])C(*)=O 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model belongs to a continuous production device for oxamide; the system comprises a dimethyl oxalate storage tank, wherein the dimethyl oxalate storage tank is connected with a product kettle through a dimethyl oxalate raw material tank; the lower part of the product kettle is a liquid phase zone, and the upper part of the product kettle is a reaction zone; a temperature control jacket is arranged outside the reaction zone, and a reflux port, a gas phase outlet and a methanol flushing port are arranged at the top of the reaction zone; an ammonia inlet connected with an ammonia storage tank is arranged on one side of the upper part of the liquid phase region, a feed opening is arranged at the bottom of the liquid phase region, a circulating liquid phase outlet is arranged on one side of the lower part of the liquid phase region, and the circulating liquid phase outlet is connected with a reflux opening through a pipeline with a dimethyl oxalate circulating pump; the device has the advantages of simple structure, reasonable design, convenience in operation, capability of accelerating the reaction process, realizing continuous production, improving the heat exchange efficiency, ensuring the normal operation of the device and avoiding the blockage of the device and the pipeline by the solid oxamide generated by the reaction.
Description
Technical Field
The utility model belongs to the technical field of oxamide production, and particularly relates to a continuous production device for oxamide.
Background
Oxamide is a white powder containing nitrogen 31.8%, has no moisture absorption in air, no toxicity and easy storage, has water solubility of 0.016%, and gradually releases ammonia nitrogen and carbon dioxide during hydrolysis or biological decomposition, and is a good urea-aldehyde slow-release fertilizer. The method for producing the oxamide is various, namely a method for preparing the oxamide by taking hydrocyanic acid as a raw material, wherein the hydrocyanic acid is extremely toxic, has higher cost and cannot realize industrialization; the other method is dimethyl oxalate ammonolysis, which comprises heating dimethyl oxalate to gas phase to react with ammonia gas to prepare oxamide, but the reaction efficiency is too low; based on the general adoption, dimethyl oxalate is dissolved in methanol to carry out ammonolysis reaction with ammonia gas to produce oxamide and methanol. The method is a gas-liquid phase intermittent reaction, and cannot realize continuous production; the specific production process is that methanol is used as solvent, liquid-phase dimethyl oxalate is placed in the solvent, ammonia gas is introduced at the same time and stands for about four hours, and the excessive ammonia gas and the dimethyl oxalate are fully reacted to produce the oxamide.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the utility model provides the continuous oxamide production device which has the advantages of simple structure, reasonable design and convenient operation, can accelerate the reaction process, realize continuous production, improve the heat exchange efficiency, ensure the normal operation of equipment and simultaneously avoid solid oxamide generated by the reaction from blocking the equipment and pipelines.
In order to achieve the purpose, the utility model adopts the technical scheme that:
a continuous production device for oxamide comprises a dimethyl oxalate storage tank, wherein the dimethyl oxalate storage tank is connected with a product kettle through a dimethyl oxalate raw material tank; the lower part of the product kettle is a liquid phase zone, and the upper part of the product kettle is a reaction zone; a temperature control jacket is arranged outside the reaction zone, and a reflux port, a gas phase outlet and a methanol flushing port are arranged at the top of the reaction zone; one side of the upper part of the liquid phase area is provided with an ammonia inlet connected with an ammonia storage tank, the bottom of the liquid phase area is provided with a feed opening, one side of the lower part of the liquid phase area is provided with a circulating liquid phase outlet, and the circulating liquid phase outlet is connected with a reflux opening through a pipeline with a dimethyl oxalate circulating pump.
Preferably, the gas phase outlet of the reaction zone in the product kettle is connected with a gas-liquid separation tank through an outlet cooler, the liquid phase of the gas-liquid separation tank is connected with a filtrate tank, the gas phase of the gas-liquid separation tank is connected with an ammonia washing tower, the top of the ammonia washing tower is connected with an emptying pipe network, and the bottom of the ammonia washing tower is connected with a dilute ammonia water storage tank through an ammonia water pump.
Preferably, a discharge opening of the liquid phase region in the product kettle is connected with a lock hopper through a discharge valve, the bottom of the lock hopper is connected with an oxamide filtering device through a lock hopper discharge valve, and a solid phase outlet of the oxamide filtering device is connected with a crude oxamide storage tank.
Preferably, a liquid phase outlet of the oxamide filtering device is connected with a filtrate tank, and an outlet of the filtrate tank is respectively connected with a lock hopper flushing port at the upper part of the lock hopper and the methanol separation and recovery unit through a filtrate pump.
Preferably, the methanol separation and recovery unit comprises a dimethyl oxalate recovery tower connected with a filtrate pump, a tower top condenser is arranged at the tower top of the dimethyl oxalate recovery tower, a tower bottom reboiler is arranged at the tower bottom of the dimethyl oxalate recovery tower, a liquid phase outlet of the dimethyl oxalate recovery tower is connected with a dimethyl oxalate stock tank, a top gas phase outlet of the dimethyl oxalate recovery tower is connected with an intermediate methanol tank, and the intermediate methanol tank is respectively connected with a methanol storage tank and a methanol flushing port of a reaction zone in a product kettle through a methanol pump.
Preferably, a nitrogen inlet connected with a nitrogen storage tank is arranged on one side of a feed opening of a liquid phase area in the product kettle, the nitrogen inlet is connected with an annular coil pipe arranged on the inner wall of the bottom of the product kettle, and an air jet is arranged on the annular coil pipe.
Preferably, a raw material pump and a raw material preheater are sequentially arranged between the dimethyl oxalate raw material tank and the product kettle.
Preferably, the upper part of the temperature control jacket is connected with a circulating water inlet pipeline, and the lower part of the temperature control jacket is connected with a circulating water return pipeline.
Preferably, a lock bucket flushing valve is arranged between the filtrate pump and a lock bucket flushing port at the upper part of the lock bucket; and a methanol flushing valve is arranged between the methanol pump and a methanol flushing port of the reaction zone in the product kettle.
Preferably, a filter screen is arranged at the outlet of the circulating liquid phase.
According to the continuous production device for the oxamide prepared by the scheme, the dimethyl oxalate dissolved in the methanol can flow from top to bottom in the reaction zone at the upper part of the product kettle through the pipeline with the dimethyl oxalate circulating pump and is contacted with the counter-current ammonia gas for reaction; the gas phase and the liquid phase can be directly and effectively contacted to achieve the purposes of accelerating the reaction and fully reacting the materials, and simultaneously, a large amount of heat generated in the reaction process is subjected to heat exchange and temperature control through a temperature control jacket to ensure the stable operation of the reaction; the reactants and the products are gas, liquid and solid, wherein the solid is easy to adhere to the inner wall of the reaction area to cause the problem of yield reduction or blockage; further, the utility model realizes gas-liquid separation by arranging the outlet cooler and the gas-liquid separation tank, and realizes the recovery of ammonia by the ammonia washing tower; in addition, the coil pipe with the air jet can prevent the solid phase from blocking the feed opening, and can realize micro stirring of the solid phase and the liquid phase in the liquid phase region so as to ensure that the materials uniformly pass through the pipeline with the dimethyl oxalate circulating pump; furthermore, in order to prevent the pipeline with the dimethyl oxalate circulating pump from being blocked, the utility model is also provided with a filter screen; in the utility model, the liquid phase material and the flushing liquid phase enter a methanol separation and recovery unit, part of methanol can be recovered in the unit, and the other part of methanol containing dimethyl oxalate can enter a product kettle for recycling through a dimethyl oxalate raw material tank; the process has the advantages of simple structure, reasonable design, convenience in operation, capability of accelerating the reaction process to realize continuous production, improving the heat exchange efficiency, ensuring the normal operation of equipment and simultaneously avoiding the blockage of the equipment and the pipeline by the solid oxamide generated by the reaction.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
FIG. 2 is a schematic diagram of the internal structure of the product tank of the present invention.
Fig. 3 is a schematic structural view of the annular coil of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, 2, 3: the utility model relates to a continuous production device for oxamide, which comprises a dimethyl oxalate storage tank 19, wherein the dimethyl oxalate storage tank 19 is connected with a product kettle 2 through a dimethyl oxalate raw material tank 20; the lower part of the product kettle 2 is a liquid phase area, and the upper part thereof is a reaction area; the outside of the reaction zone is provided with a temperature control jacket 1, and the top of the reaction zone is provided with a reflux port, a gas phase outlet and a methanol flushing port; one side of the upper part of the liquid phase area is provided with an ammonia inlet connected with an ammonia storage tank 5, the bottom of the liquid phase area is provided with a feed opening, one side of the lower part of the liquid phase area is provided with a circulating liquid phase outlet, and the circulating liquid phase outlet is connected with a reflux opening through a pipeline with a dimethyl oxalate circulating pump 3. According to the utility model, the product kettle 2 with the structure can realize the separation of liquid phase reactants and products from the reaction process, the separation can realize the sufficient contact of reaction materials in the reaction process, the reaction rate is improved, and meanwhile, the heat of the reaction zone can be rapidly removed in a targeted manner under the condition of the subareas, so that conditions are created for ensuring the long-time stable operation of equipment; the operation of the equipment can effectively shorten the reaction time, and the equipment can continue to react new materials after the materials in the solid state, the liquid state and the gas state are discharged, namely the product kettle 2 is always in a reaction state, so that the aim of continuous production is fulfilled.
Further, a gas phase outlet of the reaction zone in the product kettle 2 is connected with a gas-liquid separation tank 28 through an outlet cooler 27, a liquid phase of the gas-liquid separation tank 28 is connected with the filtrate tank 13, a gas phase of the gas-liquid separation tank 28 is connected with an ammonia washing tower 29, the top of the ammonia washing tower 29 is connected with an emptying pipe network 31, and the bottom of the ammonia washing tower 29 is connected with a dilute ammonia water storage tank 35 through an ammonia water pump 30. The gas phase in the utility model contains ammonia gas, nitrogen gas, methanol containing dimethyl oxalate and impurity gas, the gas-liquid separation can be realized by using the gas-liquid separation tank 28, the methanol containing dimethyl oxalate can be changed into liquid phase for reflux and recycling, and the ammonia in the separated gas phase is effectively recovered.
Further, a discharge opening of a liquid phase region in the product kettle 2 is connected with a lock hopper 9 through a discharge valve 8, the bottom of the lock hopper 9 is connected with an oxamide filtering device 11 through a lock hopper discharge valve 10, and a solid phase outlet of the oxamide filtering device 11 is connected with a crude oxamide storage tank 12. The utility model vacates space for the reacted materials in the product kettle 2 by arranging the lock hopper 9, ensures the long-time stable and continuous operation of the product kettle 2, and lays a foundation for the subsequent filtration of the oxamide filtration device 11. The oxamide filtering device 11 is one of a belt filter and a plate-and-frame filter press, and mainly aims to realize solid-liquid separation, wherein the solid substance is oxamide and enters a crude oxamide storage tank 12.
Further, a liquid phase outlet of the oxamide filtering device 11 is connected with a filtrate tank 13, and an outlet of the filtrate tank 13 is respectively connected with a lock hopper flushing port at the upper part of the lock hopper 9 and a methanol separation and recovery unit through a filtrate pump 14. The liquid phase filtered by the oxamide filtering device 11 enters a filtrate tank 13, one part of the liquid phase is used for recovering methanol, and the other part of the liquid phase can be used as flushing liquid of the lock hopper 9, so that the oxamide is prevented from being attached to the inner wall of the lock hopper 9 or blocking a pipeline connected with a lock hopper discharge valve 10.
Further, the methanol separation and recovery unit comprises a dimethyl oxalate recovery tower 16 connected with a filtrate pump 14, a tower top condenser 17 is arranged at the tower top of the dimethyl oxalate recovery tower 16, a tower bottom reboiler 18 is arranged at the tower bottom of the dimethyl oxalate recovery tower 16, a liquid phase outlet of the dimethyl oxalate recovery tower 16 is connected with a dimethyl oxalate raw material tank 20, a top gas phase outlet of the dimethyl oxalate recovery tower 16 is connected with an intermediate methanol tank 23, and the intermediate methanol tank 23 is respectively connected with a methanol storage tank 25 and a methanol flushing port of a reaction zone in the product kettle 2 through a methanol pump 24. The requirement of the dimethyl oxalate recovery tower 16 in the utility model is not over high, only a part of product methanol is needed to be separated, and one part of the separated methanol is used for recovering the other part of the separated methanol to be used as flushing liquid of a reaction zone in the product kettle 2; the other part of the methanol containing dimethyl oxalate separated by the dimethyl oxalate recovery tower 16 can enter the dimethyl oxalate raw material tank 20 for circular reaction, thus effectively saving the cost and improving the yield of the product.
Furthermore, a nitrogen inlet connected with the nitrogen storage tank 4 is arranged on one side of a feed opening of the liquid phase region in the product kettle 2, the nitrogen inlet is connected with an annular coil pipe 33 arranged on the inner wall of the bottom of the product kettle 2, and an air jet 34 is arranged on the annular coil pipe 33. According to the utility model, the annular coil 33 with the air jet 34 is arranged, so that on one hand, the influence on the yield caused by the attachment of solid oxamide to the inner wall of the product kettle 2 can be avoided, and on the other hand, the methanol containing dimethyl oxalate can be uniformly distributed in the liquid phase region, so that the reaction in the reaction region is ensured to be long-term, stable and efficient, and on the other hand, the liquid phase can drive the solid phase to be in a motion state all the time, so that the blockage of a feeding port by the solid oxamide in the feeding process can be avoided.
Further, a raw material pump 21 and a raw material preheater 22 are sequentially arranged between the dimethyl oxalate raw material tank 20 and the product kettle 2.
Furthermore, the upper part of the temperature control jacket 1 is connected with a circulating water inlet pipe 6, and the lower part of the temperature control jacket 1 is connected with a circulating water return pipe 7. By means of the arrangement, the temperature can be controlled in a targeted manner, and the reaction can be carried out stably.
Furthermore, a lock bucket flushing valve 15 is arranged between the filtrate pump 14 and a lock bucket flushing port at the upper part of the lock bucket 9; a methanol flushing valve 26 is arranged between the methanol pump 24 and a methanol flushing port of the reaction zone in the product kettle 2.
Further, a filter screen 32 is arranged at the outlet of the circulating liquid phase. The filter screen 32 can ensure that the circulating pump 3 with dimethyl oxalate can stably run and the nearby pipelines can not be blocked.
The working process of the utility model comprises the following steps: step 1: dimethyl oxalate in a dimethyl oxalate storage tank 19 enters a dimethyl oxalate raw material tank 20 and enters a product kettle 2 through a raw material pump 21 and a raw material preheater 22; the outlet pressure of the raw material pump 21 is 0.1-0.5 MPa; step 2: methanol in the methanol storage tank 25 enters a liquid phase region of the product kettle 2 through a methanol flushing port; after dissolving dimethyl oxalate in methanol, enabling ammonia in an ammonia storage tank 5 to enter a liquid phase region of a product kettle 2 through an ammonia inlet, then entering a reaction region, and ascending; simultaneously starting a dimethyl oxalate circulating pump 3 to ensure that the methanol containing dimethyl oxalate enters the reaction zone through a reflux opening and descends; after methanol containing dimethyl oxalate and ammonia gas are in countercurrent contact and fully react, solid oxamide is quickly generated by reaction, and a large amount of heat is generated; circulating water in the circulating water inlet pipeline 6 enters the temperature control jacket 1 to exchange heat with heat generated by the reaction for temperature control, and the circulating water after heat exchange is discharged outside through the circulating water return pipeline 7; the dimethyl oxalate circulating pump 3 continuously operates, and meanwhile, the ammonia storage tank 5 continuously supplies ammonia to the product kettle 2 to ensure that the reaction is continuously carried out, wherein the equation of the reaction is as follows:
C4H6O4(l)+2NH3(g)→(CONH2)2(s)+CH3OH(l)
the outlet pressure of the dimethyl oxalate circulating pump 3 is as follows: 0.1-0.5 MPa;
and step 3: in the process of continuously carrying out the reaction in the step 2, continuously blowing nitrogen into the bottom of the product kettle 2 by the nitrogen in the nitrogen storage tank 4 through the nitrogen inlet, the annular coil 33 and the air jet 34, so that the solid phase and the liquid phase at the bottom of the product kettle 2 are always in a micro-stirring state; simultaneously intermittently starting a methanol flushing valve 26 to flush the reaction zone of the product kettle 2, so as to avoid the defects that solid oxamide is adhered to the inner wall of the reaction zone and is blocked; the methanol flushing valve 26 is opened and closed periodically, and is opened once every 2 to 6 hours for 10 to 20 minutes each time. And 4, step 4: when the reaction in the step 2 is continuously carried out, the gas phase in the product kettle 2 is discharged, the gas phase is firstly cooled through an outlet cooler 27, and then enters a gas-liquid separation tank 28 for gas-liquid separation, secondly, the liquid phase of the gas-liquid separation enters a filtrate tank 13, the gas phase of the gas-liquid separation enters an ammonia washing tower 29 for recovering ammonia gas, and finally, the recovered ammonia gas is recovered in the form of dilute ammonia water and can be sold; and the gas phase passing through the ammonia washing tower 29 is discharged through an emptying pipe network 31. And 5: after the reaction in the step 2 is finished, the material in the product kettle 2 enters the lock hopper 9 through the feed opening and the discharge valve 8, the lock hopper 9 unloads the oxamide filtering device 11, the oxamide filtering device 11 is started to filter the material in the unloading process, and the lock hopper flushing valve 15 is opened at the same time, so that the filtrate in the filtrate tank 13 flushes the lock hopper 9. Step six: the solid material obtained by filtering by the oxamide filtering device 11 is oxamide, and enters the crude oxamide storage tank 12, and the liquid phase obtained by filtering enters the filtrate tank 13; the filtrate in the filtrate tank 13 is pressurized by a filtrate pump 14 and is respectively used for flushing the lock hopper 9 and entering a dimethyl oxalate recovery tower 16 for recovery; the outlet pressure of the filtrate pump 14 is 0.1-0.5 MPa. And 7: the filtrate enters a dimethyl oxalate recovery tower 16 and then is separated and recovered from methanol and dimethyl oxalate through a matched tower top condenser 17 and a matched tower bottom reboiler 18, and a part of methanol is condensed through the tower top condenser 17 and then enters an intermediate methanol tank 23 and is respectively sent into a product kettle 2 and a methanol storage tank 25 through a methanol pump 24; it is noted that methanol fed to product tank 2 may act as a solvent or rinse. And 8: the other part of the methanol containing dimethyl oxalate separated and recovered by the dimethyl oxalate recovery tower 16 is introduced into a dimethyl oxalate raw material tank 20 and may be fed into the product tank 2 to be re-reacted (when the methanol containing dimethyl oxalate is fed, a part of dimethyl oxalate may be replenished through a dimethyl oxalate storage tank 19). The process has the characteristics of simple structure, reasonable design, convenience in operation, capability of accelerating the reaction process to realize continuous production, improving the heat exchange efficiency, ensuring the normal operation of equipment and simultaneously avoiding the blockage of the equipment and the pipeline by the solid oxamide generated by the reaction.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A continuous production device for oxamide comprises a dimethyl oxalate storage tank (19), and is characterized in that: the dimethyl oxalate storage tank (19) is connected with the product kettle (2) through a dimethyl oxalate raw material tank (20);
the lower part of the product kettle (2) is a liquid phase area, and the upper part thereof is a reaction area; a temperature control jacket (1) is arranged outside the reaction zone, and a reflux port, a gas phase outlet and a methanol flushing port are arranged at the top of the reaction zone; one side of the upper part of the liquid phase area is provided with an ammonia inlet connected with an ammonia storage tank (5), the bottom of the liquid phase area is provided with a feed opening, one side of the lower part of the liquid phase area is provided with a circulating liquid phase outlet, and the circulating liquid phase outlet is connected with a reflux opening through a pipeline with a dimethyl oxalate circulating pump (3).
2. The continuous oxamide production apparatus as claimed in claim 1, wherein: the gas phase outlet of the reaction zone in the product kettle (2) is connected with a gas-liquid separation tank (28) through an outlet cooler (27), the liquid phase of the gas-liquid separation tank (28) is connected with a filtrate tank (13), the gas phase of the gas-liquid separation tank (28) is connected with an ammonia washing tower (29), the top of the ammonia washing tower (29) is connected with a vent pipe network (31), and the bottom of the ammonia washing tower (29) is connected with a dilute ammonia water storage tank (35) through an ammonia water pump (30).
3. The continuous oxamide production apparatus as claimed in claim 1, wherein: and a discharge opening of a liquid phase area in the product kettle (2) is connected with a lock hopper (9) through a discharge valve (8), the bottom of the lock hopper (9) is connected with an oxamide filtering device (11) through a lock hopper discharge valve (10), and a solid phase outlet of the oxamide filtering device (11) is connected with a crude oxamide storage tank (12).
4. The continuous oxamide production apparatus as claimed in claim 3, wherein: the liquid phase outlet of the oxamide filtering device (11) is connected with a filtrate tank (13), and the outlet of the filtrate tank (13) is respectively connected with a lock hopper flushing port at the upper part of the lock hopper (9) and a methanol separation and recovery unit through a filtrate pump (14).
5. The continuous oxamide production apparatus as claimed in claim 4, wherein: the methanol separation and recovery unit comprises a dimethyl oxalate recovery tower (16) connected with a filtrate pump (14), a tower top condenser (17) is arranged at the tower top of the dimethyl oxalate recovery tower (16), a tower bottom reboiler (18) is arranged at the tower bottom of the dimethyl oxalate recovery tower (16), a liquid phase outlet of the dimethyl oxalate recovery tower (16) is connected with a dimethyl oxalate stock tank (20), a top gas phase outlet of the dimethyl oxalate recovery tower (16) is connected with an intermediate methanol tank (23), and the intermediate methanol tank (23) is respectively connected with a methanol storage tank (25) and a methanol flushing port of a reaction zone in a product kettle (2) through a methanol pump (24).
6. The continuous oxamide production apparatus as claimed in claim 1, wherein: one side of a feed opening of a liquid phase area in the product kettle (2) is provided with a nitrogen inlet connected with a nitrogen storage tank (4), the nitrogen inlet is connected with an annular coil pipe (33) arranged on the inner wall of the bottom of the product kettle (2), and the annular coil pipe (33) is provided with an air jet (34).
7. The continuous oxamide production apparatus as claimed in claim 1, wherein: and a raw material pump (21) and a raw material preheater (22) are sequentially arranged between the dimethyl oxalate raw material tank (20) and the product kettle (2).
8. The continuous oxamide production apparatus as claimed in claim 1, wherein: the upper part of the temperature control jacket (1) is connected with a circulating water inlet pipeline (6), and the lower part of the temperature control jacket (1) is connected with a circulating water return pipeline (7).
9. The continuous oxamide production apparatus as claimed in claim 5, wherein: a lock bucket flushing valve (15) is arranged between the filtrate pump (14) and the lock bucket flushing port at the upper part of the lock bucket (9); a methanol flushing valve (26) is arranged between the methanol pump (24) and a methanol flushing port of the reaction zone in the product kettle (2).
10. The continuous oxamide production apparatus as claimed in claim 1, wherein: and a filter screen (32) is arranged at the outlet of the circulating liquid phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122766298.5U CN216192002U (en) | 2021-11-10 | 2021-11-10 | Continuous production device for oxamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122766298.5U CN216192002U (en) | 2021-11-10 | 2021-11-10 | Continuous production device for oxamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216192002U true CN216192002U (en) | 2022-04-05 |
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| CN115715962A (en) * | 2022-11-30 | 2023-02-28 | 赛鼎工程有限公司 | A device and method for continuous and efficient preparation of oxamide |
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