Background
The chemical name of NMP is N-methyl pyrrolidone (NMP), which is a high boiling point, environment-friendly and excellent solvent, and has the advantages of low viscosity, chemical stability, good performance and thermal stability, high polarity, low volatility, unlimited miscibility with water and many organic solvents, and the like. The market application field of the N-methyl pyrrolidone is mainly focused on industries such as lithium batteries, circuit boards, insulating materials, petrifaction, medicines, pesticides, cleaning, macromolecules and the like. NMP is produced mainly through ammonification reaction between GBL and monomethylamine.
The prior art CN201921049113.5 discloses an ammoniation reaction device for NMP production, which comprises a shell, wherein a preheating chamber and a reaction chamber are arranged in the shell, a horizontal snakelike and horizontal corrugated GBL feeding pipe and a monomethylamine feeding pipe are respectively arranged in the preheating chamber, discharge ports of the GBL feeding pipe and the monomethylamine feeding pipe are respectively connected with a reaction pipe in the reaction chamber, and the reaction pipe sequentially comprises a stabilizing section, a mixing section and a reaction section according to the direction of reaction materials; the mixing section is a spiral flat pipe, and the stabilizing section and the reaction section are linear round pipes. The device of the scheme has a simple structure, is easy to disassemble and maintain, reduces the subsequent heat load required for heating the material to the reaction temperature, and saves energy and production cost.
The scheme adopts a monomethylamine solution, so that a large amount of water in the system needs to be separated, the operation cost is increased, and the energy consumption of unit products is high; meanwhile, the sleeve is longer, so that the heat loss is larger, and the energy consumption is correspondingly increased; large-scale production is realized, the equipment investment is large, and the operation difficulty is large.
Disclosure of Invention
This scheme provides an energy-conserving NMP synthesizer.
In order to achieve the above object, the present invention provides an NMP synthesizing apparatus including: a GBL elevated tank, a monomethylamine elevated tank and a reactor; further comprising: a GBL metering pump, a monomethylamine metering pump and a static mixer; the GBL elevated tank is communicated with the GBL metering pump; the monomethylamine head tank is communicated with a monomethylamine metering pump; the GBL metering pump and the monomethylamine metering pump are both communicated with the static mixer; the reactor comprises a coil and a shell; the coil pipe is fixedly arranged in the shell; a gap is formed between the coil pipe and the shell; the coil is communicated with the static mixer; an oil inlet and an oil outlet are respectively arranged at two ends of the shell.
The principle of the scheme is as follows: the GBL raw material is introduced into a GBL elevated tank, then is conveyed into a static mixer through a GBL metering pump, and simultaneously is introduced into a monomethylamine elevated tank, wherein the monomethylamine raw material is high-purity monomethylamine, and then is conveyed into the static mixer through the monomethylamine metering pump. The static mixer fully mixes GBL and monomethylamine before entering the reactor, the fully mixed GBL and monomethylamine enter the coil pipe, heat conduction oil with the temperature set from an oil inlet of the shell is filled in a gap between the coil pipe and the shell, the coil pipe is soaked in the heat conduction oil, the GBL and monomethylamine react in the coil pipe to generate NMP, and after the GBL and monomethylamine react for the set time, materials in the coil pipe are discharged to carry out the next procedure.
The scheme has the beneficial effects that: the GBL metering pump and the monomethylamine metering pump control the raw material ratio, so that stable raw materials enter the static mixer, NMP is prepared by adopting high-purity monomethylamine, the separation of a finished product and water after reaction is reduced, and the operation cost is reduced; the water entering the coil pipe is reduced, so that the heat for heating the water is reduced, namely, the heat loss is reduced; meanwhile, the contact area of monomethylamine and GBL is enlarged by reducing water, and the reaction speed is accelerated.
Further, the coil pipe is communicated with a high-pressure buffer tank; the high-pressure buffer tank is provided with a methylamine detector and a PLC controller; the high-pressure buffer tank is provided with an exhaust hole, an electric valve is arranged at the exhaust hole, the exhaust hole is communicated with an unqualified tank, and the unqualified tank is communicated with the static mixer; the monomethylamine detector is arranged at a feed inlet of the high-pressure buffer tank and is positioned in the high-pressure buffer tank; and the PLC is electrically connected with the monomethylamine detector and the electric valve switch.
When the product in the coil pipe is discharged into the high-pressure buffer tank and the reaction is unqualified, a certain amount of monomethylamine remains in the high-pressure buffer tank, and when the monomethylamine detector detects that the concentration of the monomethylamine exceeds a set value, the PLC controller controls to open the electric valve, so that the reacted high-temperature gas is discharged into the unqualified tank and enters the static mixer again for reaction. When the concentration of the monomethylamine is lower than a set value, the PLC controller controls the electric valve to be closed. In the prior art, the product is judged to be qualified according to experience or is inspected when the product is finished, and the cost of the product is higher. Whether the finished product is qualified or not is detected by the monomethylamine detector, and the reaction is carried out again if the finished product is unqualified, so that the cost is saved, and the product yield is improved.
Further, a nitrogen inlet is arranged on the high-pressure buffer tank and communicated with a high-pressure nitrogen tank; the nitrogen inlet is communicated with a first branch pipe, and an outlet of the first branch pipe corresponds to a detection port of the monomethylamine detector; and a first electric valve is arranged in the first branch pipe, and a first electric valve switch is electrically connected with the PLC.
When the monomethylamine detector detects that the concentration of monomethylamine exceeds a set value, the PLC controller opens the first electric valve to open the first branch pipe, so that high-pressure nitrogen enters the high-pressure buffer tank from the first branch pipe, and high-pressure gas enables reaction products to completely enter the non-closed tank to prevent the products from remaining; the high-pressure gas can accelerate the reaction rate of the reaction product (for the chemical reaction with gas, when other conditions are unchanged (except volume), the pressure is increased, namely the volume is reduced, the concentration of the reactant is increased, the number of activated molecules in unit volume is increased, the effective collision times in unit time are increased, and the reaction rate is accelerated), so that the raw materials are fully reacted; meanwhile, the nitrogen washes the monomethylamine detector, so that monomethylamine is prevented from remaining on the monomethylamine detector, and the sensitivity of the monomethylamine detector is ensured.
Furthermore, the nitrogen inlet is communicated with a second branch pipe, and an outlet of the second branch pipe corresponds to a detection port of the monomethylamine detector; a second electric valve is arranged in the second branch pipe, and a switch of the second electric valve is electrically connected with the PLC; the first branch pipe and the second branch pipe are respectively positioned at two ends of a methylamine detector. When the monomethylamine detector detects that the concentration of monomethylamine exceeds a set value, the PLC is enabled to set time and intermittently switch to open the first electric valve or the second electric valve, nitrogen is enabled to flush the monomethylamine detector, the monomethylamine detector is cleaned more comprehensively, and the sensitivity of the monomethylamine detector is ensured.
Further, a methylamine mixer is arranged between the methylamine metering pump and the static mixer; a GBL mixer is arranged between the GBL metering pump and the static mixer; the monomethylamine mixer is used for providing stable materials for the monomethylamine metering pump, and can buffer the supply of system materials. The GBL mixer is used for providing stable materials for the GBL metering pump, and meanwhile, the GBL mixer can buffer the supply of the system materials.
Further, the bottom of the high-pressure buffer tank is provided with a base for supporting the buffer tank, so that the buffer tank is more stable.
Further, the high-pressure buffer tank is provided with a discharge port; the discharge outlet is provided with a flow regulating valve, so that the flow of discharged products can be conveniently regulated.
Furthermore, four oil inlets and four oil outlets are respectively arranged at two ends of the shell, so that the heat conduction oil can be rapidly filled and can uniformly flow in the tank body.
Detailed Description
The following is further detailed by the specific embodiments:
reference numerals in the drawings of the specification include: the device comprises an electric valve 1, a nitrogen inlet pipe 2, a feeding pipe 3, a discharging pipe 4, a monomethylamine detector 5, a manhole 6, a hole cover 7, a GBL elevated tank 8, a monomethylamine elevated tank 9, a GBL metering pump 10, a monomethylamine metering pump 11, a static mixer 12, a reactor 13, an oil outlet 14, an oil inlet 15, an unqualified tank 16, a high-pressure nitrogen tank 17, a high-pressure buffer tank 18, a first branch pipe 19 and a second branch pipe 20.
Example (b):
as shown in fig. 1, an NMP synthesis apparatus includes a GBL elevated tank 8, a monomethylamine elevated tank 9, a GBL metering pump 10, a monomethylamine metering pump 11, and a static mixer 12, the GBL elevated tank 8 is communicated with the GBL metering pump 10, the monomethylamine elevated tank 9 is communicated with the monomethylamine metering pump 11, and both the GBL metering pump 10 and the monomethylamine metering pump 11 are communicated with the static mixer 12. A methylamine mixer is arranged between the methylamine metering pump 11 and the static mixer 12; a GBL mixer is arranged between the GBL metering pump 10 and the static mixer 12; the monomethylamine mixer is used for providing stable materials for the monomethylamine metering pump 11 and can buffer the supply of system materials. The GBL mixer is used to stabilize the supply of material to the GBL metering pump 10 while providing a buffer effect on the supply of system material.
GBL head tank 8: GBL raw materials outside the battery limits are introduced into a GBL elevated tank 8 and then are conveyed to a GBL mixer through a GBL metering pump 10, and the GBL mixer is used for providing stable materials for the metering pump and simultaneously has a buffering effect on the supply of system materials. Monomethylamine head tank 9: the monomethylamine raw material outside the battery compartment is introduced into a monomethylamine head tank 9 and then is sent to a monomethylamine mixer through a monomethylamine metering pump 11, and the device aims to provide stable materials for the metering pump and can buffer the supply of system materials.
GBL metering pump 10: the purpose of this apparatus, which pumps the GBL in the head tank to the static mixer 12 through a metering pump, is to provide a steady flow of GBL into the reaction system and to provide sufficient pressure on the material.
Monomethylamine metering pump 11: the monomethylamine in the head tank is pumped by a metering pump to a static mixer 12, the purpose of this apparatus being to provide a steady flow of monomethylamine into the reaction system and to provide sufficient pressure on the materials.
The static mixer 12: the purpose of the static mixer 12 is to mix the GBL and monomethylamine thoroughly before entering the reactor 13, increasing the efficiency of the reaction.
Reactor 13 includes coil pipe and casing, the coil pipe is fixed to be set up in the casing, there is the clearance between coil pipe and casing, coil pipe and static mixer 12 intercommunication, the casing is equipped with oil inlet 15 and oil-out 14, oil inlet 15 and oil-out 14 all communicate with coil pipe and casing clearance, the casing left end still is connected with four oil inlets 15, four oil inlets 15 are along the circumference equipartition of casing, the casing right-hand member is connected with four oil-out 14, four oil-out 14 are equally along the circumference equipartition of casing. The arrangement enables the heat conduction oil to be rapidly filled and to uniformly flow in the tank body. The coil is communicated with a high-pressure buffer tank 18.
The GBL raw material is introduced into a GBL elevated tank 8, then is sent into a static mixer 12 through a GBL metering pump 10, and simultaneously, the monomethylamine raw material is introduced into a monomethylamine elevated tank 9, wherein the monomethylamine raw material is high-purity monomethylamine, and then is sent into the static mixer 12 through a monomethylamine metering pump 11. The static mixer 12 fully mixes GBL and monomethylamine before entering the reactor 13, the fully mixed GBL and monomethylamine enter the coil pipe, heat conduction oil with the temperature set from an oil inlet 15 of the shell is filled in a gap between the coil pipe and the shell, the coil pipe is soaked in the heat conduction oil, the GBL and monomethylamine react in the coil pipe to generate NMP, and after the GBL and monomethylamine react for a set time, materials in the coil pipe are discharged.
As shown in the attached figure 2, a methylamine detector 5 and a PLC controller are arranged on the high-pressure buffer tank 18, the model of the methylamine detector 5 is RBT-6000-ZLG, and the measurement range is 0-100 ppm. The side surface of the bottom of the high-pressure buffer tank 18 is provided with a feeding hole, and the feeding hole is communicated with a feeding pipe 3. The bottom of the high-pressure buffer tank 18 is provided with a discharge outlet which is communicated with a discharge pipe 4. The discharge outlet is provided with a flow regulating valve, so that the flow of discharged products can be conveniently regulated. The bottom of the high-pressure buffer tank 18 is provided with a base for supporting the buffer tank, so that the buffer tank is more stable. Be provided with the inspection hole on the base, the base intussuseption is filled with the heat preservation cotton, conveniently inspects high-pressure buffer tank 18 and reduces reaction product heat and runs off.
The high-pressure buffer tank 18 is provided with an exhaust hole, the exhaust hole is provided with an electric valve 1 and communicated with an unqualified tank 16, the unqualified tank 16 is communicated with the static mixer 12, the monomethylamine detector 5 is arranged at the feed inlet of the high-pressure buffer tank 18, and the monomethylamine detector 5 is positioned in the high-pressure buffer tank 18. The PLC is electrically connected with the monomethylamine detector 5 and the electric valve 1. When the product in the coil pipe is discharged into the high-pressure buffer tank 18 and the reaction is unqualified, a certain amount of monomethylamine remains in the high-pressure buffer tank 18, and when the monomethylamine detector 5 detects that the concentration of the monomethylamine exceeds a set value, the PLC controller controls the opening of the electric valve 1, so that the reacted high-temperature gas is discharged into the unqualified tank and enters the static mixer 12 again for reaction. When the monomethylamine detector 5 cannot detect monomethylamine, the PLC controller controls to close the electric valve 1. In the prior art, the product is judged to be qualified according to experience or is inspected when the product is finished, and the cost of the product is higher. Whether the finished product is qualified or not is detected by the monomethylamine detector 5, and the reaction is carried out again if the finished product is unqualified, so that the finished product is saved, and the product yield is improved.
Be equipped with the nitrogen gas air inlet on the high pressure buffer tank 18, nitrogen gas air inlet intercommunication has high-pressure nitrogen gas jar 17, nitrogen gas air inlet intercommunication has nitrogen gas intake pipe 2, nitrogen gas intake pipe 2 is located inside high pressure buffer tank 18, 2 intercommunications of nitrogen gas intake pipe have first branch pipe 19 and second branch pipe 20, first branch pipe 19 is located methylamine detector 5 upper and lower ends respectively with second branch pipe 20, 19 exports of first branch pipe and second branch pipe 20 all corresponding with methylamine detector 5 detection port, be equipped with first electric valve in the first branch pipe 19, first electric valve switch is connected with the PLC controller electricity. A second electric valve is arranged in the second branch pipe 20, and the switch of the second electric valve is electrically connected with the PLC.
When the monomethylamine detector 5 detects that the concentration of monomethylamine exceeds a set value, the PLC intermittently switches to open the first electric valve or the second electric valve within a set time, high-pressure nitrogen enters the high-pressure buffer tank 18 from the first branch pipe 19 or the second branch pipe 20 to flush the monomethylamine detector 5, and the first branch pipe 19 or the second branch pipe 20 is intermittently started to be opened to more completely clean the monomethylamine detector 5, so that the sensitivity of the monomethylamine detector 5 is ensured; the high-pressure nitrogen makes the reaction product completely enter the non-closed tank to prevent the product from remaining; the high-pressure nitrogen can accelerate the reaction rate of the reaction product (for the chemical reaction with gas, when other conditions are unchanged (except volume), the pressure is increased, namely the volume is reduced, the concentration of the reactant is increased, the number of activated molecules in unit volume is increased, the effective collision times in unit time are increased, and the reaction rate is accelerated), so that the raw materials are fully reacted.
Be equipped with manhole 6 on the 18 lower extreme lateral wall of high-pressure buffer tank, be equipped with handhole door 7 on the manhole 6, manhole 6 passes through bolt fixed connection with handhole door 7, and when manhole 6 was used for sharp superpressure or vacuum in the one-tenth jar, the prevention damaged the storage tank and the emergence accident, can play the safe back-fire relief effect again.
The operation method of the scheme comprises the following steps: the GBL raw material is introduced into a GBL elevated tank 8, then is sent into a static mixer 12 through a GBL metering pump 10, and simultaneously, the monomethylamine raw material is introduced into a monomethylamine elevated tank 9, wherein the monomethylamine raw material is high-purity monomethylamine, and then is sent into the static mixer 12 through a monomethylamine metering pump 11. The method comprises the steps that a static mixer 12 fully mixes GBL and monomethylamine before the GBL and the monomethylamine enter a coil pipe, heat conduction oil with the temperature set from an oil inlet 15 of a shell is filled in gaps between the coil pipe and the shell, the coil pipe is soaked in the heat conduction oil, the GBL and the monomethylamine react in the coil pipe to generate NMP, after the GBL and the monomethylamine react for 4-6 hours, materials in the coil pipe are discharged, after products in the coil pipe are discharged into a high-pressure buffer tank 18, when the reaction is unqualified, a certain amount of monomethylamine remains in the high-pressure buffer tank 18, and when a monomethylamine detector 5 detects that the concentration of the monomethylamine exceeds a set value of 1ppm, a PLC controller controls to open an electric valve 1, so that high-temperature gas after the reaction is discharged into an unqualified tank, and then the high-temperature gas enters the static mixer 12. The PLC is enabled to set 3S intermittent switching to open the first electric valve or the second electric valve, high-pressure nitrogen enters the high-pressure buffer tank 18 through the first branch pipe 19 or the second branch pipe 20, the high-pressure nitrogen washes the monomethylamine detector 5, the monomethylamine detector 5 is cleaned more comprehensively, and the sensitivity of the monomethylamine detector 5 is ensured; the high pressure nitrogen gas completely entered the reaction product into the autoclave. When the monomethylamine detector 5 detects that the concentration of the monomethylamine is lower than the set value by 1ppm, the PLC controller controls the electric valve 1 and the high-pressure nitrogen tank 17 to be closed, and then controls the flow regulating valve to discharge a reaction product to the next procedure. This scheme has adopted high-purity monomethylamine preparation NMP, has reduced finished product and moisture separation after the reaction, has reduced the running cost, and the water that gets into in the coil pipe reduces, has reduced the heat to the water heating, has reduced heat loss promptly, makes monomethylamine and GBL area of contact grow simultaneously for reaction rate. High-pressure nitrogen is flushed into the high-pressure buffer tank 18, the high-pressure nitrogen enables reaction products to completely enter the non-closed tank, product residues are prevented, the ammonia gas detector can be cleaned, and meanwhile, the high-pressure nitrogen plays a role in pressurizing, synthesis reaction is promoted, and the reaction is complete.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.