CN115745743A - Production process of liquid sodium methoxide - Google Patents

Production process of liquid sodium methoxide Download PDF

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Publication number
CN115745743A
CN115745743A CN202211481106.9A CN202211481106A CN115745743A CN 115745743 A CN115745743 A CN 115745743A CN 202211481106 A CN202211481106 A CN 202211481106A CN 115745743 A CN115745743 A CN 115745743A
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China
Prior art keywords
air outlet
gas
outlet pipe
pipe
tower body
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CN202211481106.9A
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Chinese (zh)
Inventor
钟友政
宋衍
宋振义
宋莹莹
陈伟伟
段高英
潘娟娟
宋长广
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Henan Shenghongfeng Chemical Co ltd
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Henan Shenghongfeng Chemical Co ltd
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Priority to CN202211481106.9A priority Critical patent/CN115745743A/en
Publication of CN115745743A publication Critical patent/CN115745743A/en
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Abstract

The invention discloses a production process of liquid sodium methoxide, which comprises the following steps: injecting a sodium hydroxide solution with the mass fraction of 22% and an anhydrous methanol solution into the tower body from a feed inlet, wherein the molar ratio of the methanol solution to the sodium hydroxide solution is 4.4, then starting an electric heater to heat the tower body, wherein the heating temperature meets 100-120 ℃, and starting a motor to stir; the water produced in the reaction process is heated and evaporated into steam, the steam is discharged from an air outlet pipe at the top of the tower body along with the volatile gas of the methanol, then the steam is pressurized by a pressurizing unit, the temperature is raised and the steam is fully vaporized, the flow rate of the mixed gas is detected by a gas flow rate detection unit, the flow rate of the gas is obtained according to the flow rate of the gas, and the consumption of the molecular sieve raw material in the separation mechanism is determined according to the flow rate of the mixed gas; the tail gas after passing through the separation mechanism enters a filtering mechanism, and the filtering mechanism comprises a filtering body provided with dilute hydrochloric acid.

Description

Production process of liquid sodium methoxide
Technical Field
The invention belongs to the technical field of sodium methoxide production, and particularly relates to a production process of liquid sodium methoxide.
Background
The traditional production method of sodium methoxide comprises a metal sodium method and an alkali method, wherein the metal sodium method is to prepare sodium methoxide by reacting metal sodium and sodium hydroxide with methanol, but the metal sodium is expensive, a large amount of heat is generated in the reaction process, hydrogen is generated in the process, and dangerous accidents are easy to occur in the operation process, so the method is not suitable for large-scale production at present.
However, in the process of producing sodium methoxide by the alkaline method, because the reaction is a reversible reaction, if water generated by the reaction is not treated timely, the reverse reaction occurs, the reaction does not completely affect the production process of sodium methoxide, and the generated sodium methoxide liquid contains water and sodium hydroxide impurities, so that the purity of sodium methoxide is low; for the currently generally adopted method, anhydrous methanol and sodium hydroxide solution are added from the upper part of a tower body, methanol steam is filled from the lower part of the tower body, water vapor generated by the reaction is carried out, methanol and water are separated through condensation and rectification, the process is complex, large-scale equipment is required to be excessive, the production yield is high, the temperature, the pressure, the feeding ratio and the feeding amount of the methanol steam need to be strictly controlled, if the methanol steam inflow is excessive, the pressure of the tower body is high, liquid interception is easy to form, if the methanol steam inflow is too small, insufficient steam-liquid contact can be caused, and the water content of the generated sodium methoxide solution is too high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a production process of liquid sodium methoxide, which is improved on the basis of the prior art, the generated mixed gas of methanol and water vapor is heated and further vaporized by arranging a pressurizing unit to form a molecular structure, and then the flow of the mixed gas is obtained by detecting the flow rate of the mixed gas by arranging a gas flow rate detection unit, so that the content of a molecular sieve in a set separation mechanism is facilitated, the aim of completely removing moisture is fulfilled, resources are reasonably configured, and excessive waste of the resources is prevented; and adsorb the processing through setting up filtering mechanism to tail gas, reduce pollution, at the inside automatic sealing mechanism that sets up of filtering mechanism, when changing the filter body, reach sealed effect automatically, tail gas leakage when preventing to change the filter body causes environmental hazard.
The invention provides the following technical scheme:
step one, injecting a sodium hydroxide solution with the mass fraction of 22% and an anhydrous methanol solution into a tower body from a feed inlet, wherein the molar ratio of the methanol solution to the sodium hydroxide solution is 4.4, then starting an electric heater to heat the tower body, the heating temperature is 100-120 ℃, and starting a motor to stir;
step two, water generated in the reaction process is heated and evaporated into steam, the steam is discharged from an air outlet pipe at the top of the tower body along with the volatile gas of the methanol, then the steam is pressurized by a pressurizing unit, the temperature is raised and the steam is fully vaporized, the flow rate is detected by a gas flow rate detection unit, the flow rate of the gas is obtained according to the flow rate of the gas, and the consumption of the molecular sieve raw material in the separation mechanism is determined according to the flow rate of the mixed gas, so that the water molecules in the methanol are completely adsorbed and removed after passing through the separation mechanism, the methanol solution enters the tower body from a new return pipe for reaction, the water generated in the tower body is better removed, the reaction is promoted to be carried out in the direction of generating the sodium methoxide, the reverse reaction is prevented, and the purity of the obtained liquid sodium methoxide is improved;
and step three, enabling the tail gas after passing through the separation mechanism to enter a filtering mechanism, wherein the filtering mechanism comprises a filtering body provided with dilute hydrochloric acid, and a small amount of methanol, sodium hydroxide and sodium methoxide contained in the tail gas can react through the arranged filtering body containing the dilute hydrochloric acid to reduce tail gas pollution.
Preferably, the production process adopts a production device comprising a tower body, wherein a motor is arranged at the bottom of the tower body, an output shaft of the motor penetrates through the bottom of the tower body, the output shaft of the motor is connected with a stirrer, the stirrer is connected with the tower body in a sealing and rotating manner, an electric heater is arranged on the side wall of the tower body, the top of the tower body is connected with an air outlet pipe, one end, close to the tower body, of the air outlet pipe is provided with a pressurizing unit, the pressurizing unit pressurizes gas in the air outlet pipe, the other end of the pressurizing unit is provided with a gas flow velocity detection unit, the gas flow velocity detection unit is arranged inside the air outlet pipe, the other end of the air outlet pipe is connected with the upper end of a separation mechanism, the bottom of the separation mechanism is connected with a return pipe, the other end of the return pipe is communicated with the tower body, the side wall, close to the bottom, of the separation mechanism is connected with a filter mechanism, and the other end of the filter mechanism is connected with a tail gas pipe; the tower body is equipped with the feed inlet near the position of top, and the tower body is equipped with the discharge gate near the position of bottom.
Preferably, the supercharging mechanism comprises a vertical shaft wind wheel, the vertical shaft wind wheel is arranged inside the air outlet pipe, rotating shafts are arranged on two sides of the vertical shaft wind wheel and penetrate through the wall of the air outlet pipe, the rotating shafts are in sealed rotating connection with the wall of the air outlet pipe, cams are connected to the rotating shafts on two sides of the vertical shaft wind wheel, the other side of each cam is in rotating connection with a connecting rod, and the other end of each connecting rod is in rotating connection with a telescopic rod; the two sides of the air outlet pipe are provided with sealing box bodies, the other end of the telescopic rod extends into the sealing box bodies, the telescopic rod and the sealing box bodies are in sealing sliding connection through the arranged rubber pads, and the other end of the telescopic rod is connected with a piston plate; one side of the sealed box body, which is far away from the telescopic rod, is provided with an increasing piece, a round hole is formed in the center of the pressurizing piece, the diameter of the air outlet pipe is reduced, one side of the sealed box body, which is far away from the air outlet pipe, is connected with an air guide pipe, and the other end of the air guide pipe is communicated with the pressurizing piece.
Preferably, a partition plate is arranged in the sealed box body, the piston plate and the outer side wall of the air outlet pipe slide in a sealing manner with the partition plate, and the air outlet pipe is of a cuboid structure; one end, close to the vertical shaft wind wheel, of the air outlet pipe, which is positioned in the sealed box body, is provided with a first air inlet, one end, close to the pressurizing piece, of the air outlet pipe is provided with a second air inlet, one side, close to the vertical shaft wind wheel, of the partition board is provided with a first air outlet, and one side, close to the pressurizing piece, of the partition board is provided with a second air outlet; the first air inlet and the second air inlet are both provided with inlet valves, the inlet valves are connected with the outer side wall of the air outlet pipe in a rotating mode through hinges, the first air outlet and the second air outlet are both provided with air outlet valves, and the air outlet valves are connected with one side, away from the piston plate, of the partition plate through the hinges in a rotating mode.
Preferably, the gas flow rate detection unit includes a pipe body, the pipe body is arranged in the outlet duct, fan blades are arranged in the pipe body, bearings are arranged at two ends of the pipe body, a supporting rod is connected to the outer side of each bearing, the other end of the supporting rod is connected with the inner side wall of the outlet duct, and the pipe body rotates through the arranged bearings.
Preferably, four rows of shifting blocks are uniformly arranged on the outer side wall of the pipe body along the circumferential direction of the pipe body, and a plurality of non-row shifting blocks are arranged; four rows of piezoelectric patches are vertically arranged on the inner wall of the tube body, the number of each row of piezoelectric patches is the same as that of the poking blocks, and the poking blocks can interfere with the piezoelectric patches when the tube body rotates; the piezoelectric patches are connected in series through wires and connected with a rectifier, and the rectifier is connected with a display instrument.
Preferably, the filtering mechanism comprises a shell, one side, close to the separating mechanism, inside the shell is connected with a fixed block, the other side of the fixed block is connected with a first spring, the other end of the first spring is connected with a moving plate, and the other side of the moving plate, close to the middle, is connected with a trapezoidal block; the movable plate is characterized in that a baffle is arranged on one side, away from the fixed block, of the movable plate, the outer side of the baffle is connected with the shell, the central position of the baffle is of a hollow structure, and the movable plate can be in sealed pressure connection with the baffle through an arranged rubber ring.
Preferably, fixing boxes are symmetrically arranged on two sides of one end, far away from the fixing block, in the shell, through grooves are formed in the side walls of the fixing boxes, guide rods are arranged in the fixing boxes, sliding rings are arranged on the guide rods, the sliding rings and the guide rods are in sliding connection, the sliding rings are connected with connecting rods, the connecting rods are arranged in the through grooves, and the connecting rods and the through grooves are in sliding connection; and a spring is arranged on the guide rod, one end of the spring is connected with the sliding ring, and the other end of the spring is connected with the inner wall of the sealing box.
Preferably, the other end of the connecting rod is connected with a clamping block, the clamping block is of a U-shaped structure, the clamping block is movably clamped with a filtering body, and dilute hydrochloric acid solution is arranged inside the filtering body; the shell is provided with a movable door, and the filter body can be taken out from the movable door for replacement.
Preferably, the separation mechanism is internally provided with a plurality of layers of molecular sieves, and the molecular sieve is a 3A molecular sieve consisting of sodium aluminosilicate or sodium calcium aluminosilicate.
Preferably, as the diameter of the water molecule is less than 3A, the critical diameter of the methanol molecule is 4.4A, the 3A molecular sieve is selected to enable the water molecule to be adsorbed through the pore diameter, the methanol molecule is blocked outside the water molecule and can not be adsorbed by the water molecule, and the water molecule flows into the tower body again from the bottom of the separation mechanism for reaction after being liquefied by temperature reduction.
In addition, through the arranged supercharging mechanism, when supercharging is carried out, the vertical axis wind wheel in the air outlet pipe rotates through the blowing of the mixed gas, the vertical axis wind wheel drives the cam and the connecting rod to rotate in the rotating process, and the connecting rod further drives the telescopic rod and the piston plate to reciprocate in the sealing box body; when the piston plate moves towards the direction close to the vertical shaft wind wheel, the inlet valve of the first air inlet is subjected toThe pressure action is closed, the inlet valve of the air inlet II is opened under the action of negative pressure, and the air in the air outlet pipe quickly enters a right pressure cavity formed by the air outlet pipe and the partition plate from the air inlet II; meanwhile, the air outlet door of the first air outlet is opened under pressure, the air outlet door of the second air outlet is closed under the action of negative pressure, and air in a left pressure cavity formed by the air outlet pipe and the partition plate quickly enters the air guide pipe from the first air outlet and enters the pressurizing piece through the air guide pipe to be subjected to secondary pressurization, so that the pressure of mixed air is increased; when the piston plate moves reversely, the action principle is the same as the above, air is fed from the air inlet I, and air is discharged from the air outlet II; from this can be incessant let gas get into the pressure boost piece from the air duct, carry out the secondary pressure boost, at the in-process of pressure boost, not only improved mist's temperature, make its vaporization more abundant, become the molecular form, be favorable to subsequent abundant separation, through the velocity of flow that improves mist moreover, help carrying out the separation of methyl alcohol and vapor more high-efficiently, improve separation efficiency to further improve production efficiency. In order to improve the supercharging effect, the stress area S of the vertical axis wind wheel cannot be too large or too small, the stress area is too large, the wind force to be pushed is too large, the airflow resistance in the air outlet pipe is too large, attenuation is caused, supercharging is not facilitated, and if the stress area is too small, the piston plate cannot be driven to reciprocate; therefore, the following relations are satisfied between the stress area S of the vertical axis wind wheel, the gas flow velocity v1 before pressurization, the gas flow velocity v2 after pressurization, the diameter r1 of the air outlet pipe and the inner diameter r2 of the pressurizing piece: s = δ (r 1-r 2) (v 1v 2/(v 1-v 2)) 1/2 (ii) a In the above formula, the unit of S is cm 2 (ii) a r1 and r2 are in the unit of cm; v1 and v2 unit is ml/min; delta is a relation coefficient, and the value range is 6.35-16.87.
In addition, when the gas flow velocity detection unit detects, mixed gas pressurized by the pressurization unit quickly enters the tube body, the inner diameter of the tube body is the same as the inner diameter of the pressurization part, after airflow enters the tube body, the fan blades arranged in the tube body are driven, the rotation of the fan blades drives the tube body to rotate, when the tube body rotates, the poking blocks arranged outside the tube body interfere with the piezoelectric sheets, the poking blocks poke the piezoelectric sheets to vibrate, and when the piezoelectric sheets vibrate, the mixed gas quickly enters the tube bodyThe two ends of the piezoelectric sheet generate potential difference, the potential difference is connected with the rectifier through the lead to be rectified to form stable current, the magnitude of the current is displayed through the connected display instrument, the magnitude of the current is in direct proportion to the flow velocity of gas, the faster the flow velocity is, the faster the rotation frequency of the tube body is, the larger the vibration amplitude and the faster the frequency of the piezoelectric sheet are, the larger the generated potential difference is, and the larger the current is; therefore, the flow velocity and the flow of the mixed gas flow can be directly reflected through the generated current, the reasonable setting of the molecular sieve in the separating mechanism is convenient to control, the purpose of completely removing the water is achieved, and resources are reasonably allocated. In order to further improve the accuracy of the dosage of the molecular sieve and prevent the excessive waste of resources, the mass M1 of the molecular sieve and the gas flow velocity v2 after pressurization, the inner diameter r2 of the pressurization piece, the working time t and the mass M2 of the water absorbing mixed gas meet the requirements that M1= lambda.2 (v 2 pi r 2) 2 t)/M2•10 3 kg/m 3 (ii) a In the above formula, the unit of M1 and M2 is g, and λ is a relation adjusting coefficient, and the value range is 0.92-1.63. Meanwhile, in order to prevent the piezoelectric sheet from being broken in the using process, ensure the using stability of the piezoelectric sheet and increase the using fatigue, the thickness b and the length L of the piezoelectric sheet meet the requirements of the Shore hardness H and the rebound resilience k of the piezoelectric sheet and the gas flow velocity v2 after pressurization, and L/b = beta (H-3 v 2) k; in the above formula, L, b unit cm, beta is the adjusting coefficient, and the value range is 1.66-3.27.
In addition, when the filter body is replaced by the filter mechanism, when the filter body is positioned in the buckle, the buckle is tightly propped against the baffle due to the elastic force of the second spring, so that sealing is formed, meanwhile, the filter body presses the trapezoidal block, the trapezoidal block props open the moving plate, the moving plate is separated from the baffle, a passage is formed, and tail gas on the left side of the filter body can be filtered by the filter body and is discharged through the tail gas pipe; when the filter body needs to be replaced, in order to prevent the filter body from being drawn out, toxic methanol tail gas is directly discharged without being filtered, so that the environment is polluted and the harm is caused to workers; when the filtering body is taken out, because the filtering body breaks away from with the trapezoidal piece, the trapezoidal piece no longer receives the pressure of filtering the body, and first spring passes through the effect of elasticity with the movable plate crimping on the baffle to closely the crimping through the rubber ring between baffle and the movable plate, form the closed circuit, when preventing to take out the filtering body, the tail gas that contains a small amount of methyl alcohol is direct to be discharged from the tail gas pipe not adsorbing, prevents to cause air pollution, the security that lifting means used. In order to prevent the filter body from being separated from the baffle plate in the inserting process, the gas overflows from the gap between the buckle and the baffle plate to the tail gas pipe, the sealing performance is further improved, and the elastic force F2 of the second spring and the elastic force F1 of the first spring meet the following requirements: f2>2F1.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the production process of the liquid sodium methoxide, the pressurizing unit is arranged, so that the temperature of the mixed gas is increased in the pressurizing process, the mixed gas is more fully vaporized and becomes in a molecular form, the subsequent full separation is facilitated, the separation of methanol and water vapor is more efficiently carried out by increasing the flow rate of the mixed gas flow, the separation efficiency is improved, and the production efficiency is further improved.
(2) According to the production process of the liquid sodium methoxide, the airflow velocity detection unit is arranged, the flow velocity and the flow of the mixed airflow can be directly reflected according to the generated current, the reasonable setting of the molecular sieve in the separation mechanism is conveniently controlled, the purpose of completely removing the moisture is achieved, and resources are reasonably allocated.
(3) According to the production process of the liquid sodium methoxide, the filtering mechanism is arranged, when the filtering body is pulled out, the filtering body is separated from the trapezoidal block, the trapezoidal block is not stressed by the pressure of the filtering body, the first spring presses the moving plate onto the baffle plate under the action of elasticity, and the baffle plate and the moving plate are tightly pressed by the rubber ring to form a closed circuit.
(4) According to the production process of the liquid sodium methoxide, the pressurization effect is improved by limiting the relationship among the stress area of the vertical axis wind wheel, the gas flow rate before pressurization, the gas flow rate after pressurization, the diameter of the gas outlet pipe and the inner diameter of the pressurization piece, the too large or too small stress area of the vertical axis wind wheel is prevented, and the piston plate is driven to reciprocate better.
(5) According to the production process of the liquid sodium methoxide, the accuracy of the using amount of the molecular sieve is further improved and excessive waste of resources is prevented by limiting the relationship between the mass of the molecular sieve and the gas flow rate after pressurization, the inner diameter of a pressurization piece, the working time and the mass of the absorbed mixed gas water.
(6) According to the production process of the liquid sodium methoxide, the piezoelectric sheet is prevented from being broken in the using process by limiting the thickness of the piezoelectric sheet and the relation between the length of the piezoelectric sheet, the Shore hardness and the rebound resilience of the piezoelectric sheet and the gas flow rate after pressurization, the use stability of the piezoelectric sheet is ensured, and the use fatigue is increased.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a flow chart of the method of the present invention.
FIG. 2 is a schematic view of the entire production apparatus of the present invention.
Fig. 3 is a schematic structural diagram of the pressurizing unit of the present invention.
Fig. 4 is a partially enlarged schematic view of the pressurizing unit of the present invention.
Fig. 5 is a schematic structural view of a gas flow rate detection unit according to the present invention.
Fig. 6 is a schematic cross-sectional view of a gas flow rate detecting unit of the present invention.
Fig. 7 is a schematic illustration of a filter body insertion configuration of the filter mechanism of the present invention.
Fig. 8 is a schematic view of a filter body removing structure of the filter mechanism of the present invention.
Fig. 9 is a schematic view of the trapezoidal block structure of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described in detail and completely with reference to the accompanying drawings. It is to be understood that the described embodiments are only a few, but not all embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Thus, the following detailed description of the embodiments of the present invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The first embodiment is as follows:
referring to fig. 1, a production process of liquid sodium methoxide is characterized by comprising the following steps of firstly, injecting a sodium hydroxide solution with the mass fraction of 22% and an anhydrous methanol solution into a tower body from a feed inlet, wherein the molar ratio of the methanol solution to the sodium hydroxide solution is 4.4, then starting an electric heater to heat the tower body, wherein the heating temperature is 100-120 ℃, and starting a motor to stir;
step two, water generated in the reaction process is heated and evaporated into steam, the steam is discharged from an air outlet pipe at the top of the tower body along with the volatile gas of the methanol, then the steam is pressurized by a pressurizing unit, the temperature is raised, the steam is fully vaporized, the flow rate is obtained by a gas flow rate detection unit, the flow rate of the gas is obtained according to the flow rate of the gas, and the consumption of the raw materials of the molecular sieve in the separation mechanism is determined according to the flow rate of the mixed gas, so that the water molecules in the methanol are completely adsorbed and removed after passing through the separation mechanism, the methanol solution enters the tower body from a new return pipe for reaction, the water generated in the tower body is better removed, the reaction is promoted to be carried out in the direction of generating the sodium methoxide, the reverse reaction is prevented, and the purity of the obtained liquid sodium methoxide is improved;
and step three, the tail gas after passing through the separation mechanism enters a filtering mechanism, the filtering mechanism contains a filtering body provided with dilute hydrochloric acid, a small amount of methanol, sodium hydroxide and sodium methoxide contained in the tail gas can react through the filtering body containing the dilute hydrochloric acid, the tail gas pollution is reduced, an automatic sealing mechanism is arranged, when the filtering body is replaced, the sealing effect is automatically achieved, and the tail gas leakage and the environmental pollution caused by the replacement of the filtering body are prevented.
Example two:
referring to fig. 2-4, on the basis of the first embodiment, the production process adopts a production apparatus including a tower body 1, a motor 2 is disposed at the bottom of the tower body 1, an output shaft of the motor 2 penetrates through the bottom of the tower body 1, an output shaft of the motor 2 is connected to a stirrer 3, the stirrer 3 is connected to the tower body 1 in a sealing and rotating manner, an electric heater 4 is disposed on a side wall of the tower body 1, an air outlet pipe 5 is connected to the top of the tower body 1, a pressurizing unit 6 is disposed at one end of the air outlet pipe 5 close to the tower body 1, the pressurizing unit 6 pressurizes air in the air outlet pipe 5, an air flow rate detecting unit 7 is disposed at the other end of the pressurizing unit 6, the air flow rate detecting unit 7 is disposed inside the air outlet pipe 5, the other end of the air outlet pipe 5 is connected to the upper end of a separating mechanism 8, a return pipe 13 is connected to the bottom of the separating mechanism 8, the other end of the return pipe 13 is communicated with the tower body 1, a filtering mechanism 9 is connected to the side wall of the separating mechanism 8 close to the bottom, and the other end of the filtering mechanism 9 is connected to a tail gas pipe 10; a feeding hole 11 is formed in the position, close to the top, of the tower body 1, and a discharging hole 12 is formed in the position, close to the bottom, of the tower body 1.
The supercharging mechanism comprises a vertical shaft wind wheel 61, the vertical shaft wind wheel 61 is arranged inside the air outlet pipe 5, rotating shafts are arranged on two sides of the vertical shaft wind wheel 61 and penetrate through the wall of the air outlet pipe 5, the rotating shafts are connected with the wall of the air outlet pipe 5 in a sealing and rotating mode, cams 62 are connected with the rotating shafts on two sides of the vertical shaft wind wheel 61, the other side of each cam 62 is connected with a connecting rod 63 in a rotating mode, and the other end of each connecting rod 63 is connected with an expansion rod 64 in a rotating mode; two sides of the air outlet pipe 5 are provided with a sealing box body 65, the other end of the telescopic rod 64 extends into the sealing box body 65, the telescopic rod 64 and the sealing box body 65 form a sealing sliding connection through an arranged rubber pad, and the other end of the telescopic rod 64 is connected with a piston plate 66; the side of the sealing box body 65, which is far away from the telescopic rod 64, is provided with an increasing piece, the center of the increasing piece 68 is provided with a round hole, the diameter of the air outlet pipe 5 is reduced, one side of the sealing box body 65, which is far away from the air outlet pipe 5, is connected with an air duct 67, and the other end of the air duct 67 is communicated with the increasing piece 68.
A partition plate 613 is arranged in the sealing box body 65, the piston plate 66 and the outer side wall of the air outlet pipe 5 slide in a sealing manner with the partition plate 613, and the air outlet pipe 5 is of a rectangular parallelepiped structure; one end, close to the vertical axis wind wheel 61, of the outlet pipe 5, which is located inside the sealed box body 65, is provided with a first air inlet 69, one end, close to the pressurizing piece 68, is provided with a second air inlet 610, one side, close to the vertical axis wind wheel 61, of the partition 613 is provided with a first air outlet 611, and one side, close to the pressurizing piece, of the partition 613 is provided with a second air outlet 612; the first air inlet 69 and the second air inlet 610 are both provided with inlet valves, the inlet valves are rotatably connected with the outer side wall of the air outlet pipe 5 through hinges, the first air outlet 611 and the second air outlet 612 are both provided with outlet valves, and the outlet valves are rotatably connected with one side, away from the piston plate 66, of the partition plate 613 through the hinges.
And a plurality of layers of molecular sieves are arranged in the separating mechanism 8, and the molecular sieve is a 3A molecular sieve consisting of sodium aluminosilicate or sodium calcium aluminosilicate.
Because the diameter of the water molecule is less than 3A, the critical diameter of the methanol molecule is 4.4A, the 3A molecular sieve can absorb the water molecule through the pore diameter, the methanol molecule is blocked outside the water molecule and can not be absorbed by the water molecule, and the water molecule flows into the tower body 1 again from the bottom of the separation mechanism 8 for reaction after being liquefied at a reduced temperature.
Through the arranged supercharging mechanism, when supercharging is carried out, the vertical shaft wind wheel 61 in the air outlet pipe 5 rotates through the blowing of mixed gas, the vertical shaft wind wheel 61 drives the cam 62 and the connecting rod 63 to rotate in the rotating process, and the connecting rod 63 further drives the telescopic rod 64 and the piston plate 66 to reciprocate in the sealed box body 65; when the piston plate 66 moves towards the direction close to the vertical shaft wind wheel 61, the inlet valve of the first air inlet 69 is closed under the action of pressure, and the second air inlet is closedThe inlet valve of 610 is opened under the action of negative pressure, and the gas in the outlet pipe 5 rapidly enters the right pressure cavity formed by the outlet pipe 5 and the partition plate 613 from the second inlet port 610; meanwhile, the air outlet door of the first air outlet 611 is opened under pressure, the air outlet door of the second air outlet 612 is closed under the action of negative pressure, air in a left pressure cavity formed by the air outlet pipe 5 and the partition plate 613 quickly enters the air guide pipe 67 from the first air outlet 611, enters the pressurizing piece 68 through the air guide pipe 67 and is pressurized for the second time, and the pressure of mixed air is increased; when the piston plate 66 moves reversely, the air is fed from the first air inlet 69 and discharged from the second air outlet 612 according to the same action principle; from this can be incessant let gas from air duct 67 entering pressure boost 68, carry out the secondary pressure boost, at the in-process of pressure boost, not only improved mist's temperature, make its vaporization more abundant, become the molecular form, be favorable to subsequent abundant separation, moreover through the velocity of flow that improves mist, help carrying out the separation of methyl alcohol and vapor more high-efficiently, improve separation efficiency to further improve production efficiency. In order to improve the supercharging effect, the stressed area S of the vertical axis wind wheel 61 cannot be too large or too small, the stressed area is too large, the wind force to be pushed is too large, the airflow resistance in the air outlet pipe 5 is too large, attenuation is caused, supercharging is not facilitated, and if the stressed area is too small, the piston plate 66 cannot be driven to reciprocate; therefore, the following relations are satisfied between the stressed area S of the vertical axis wind wheel 61, the gas flow velocity v1 before pressurization, the gas flow velocity v2 after pressurization, the diameter r1 of the gas outlet pipe 5 and the inner diameter r2 of the pressurizing part 68: s = δ (r 1-r 2) (v 1v 2/(v 1-v 2)) 1/2 (ii) a In the above formula, the unit of S is cm 2 (ii) a r1 and r2 are in the unit of cm; v1 and v2 are in the unit of ml/min; delta is a relation coefficient, and the value range is 6.35-16.87.
Example three:
as shown in fig. 5 to 6, on the basis of the first embodiment, the gas flow velocity detection unit 7 includes a pipe body 71, the pipe body 71 is disposed inside the outlet pipe 5, the inside of the pipe body 71 is provided with the fan blades 72, both ends of the pipe body 71 are provided with bearings 74, the outer side of the bearings 74 is connected with a support rod 73, the other end of the support rod 73 is connected with the inner side wall of the outlet pipe 5, and the pipe body 71 rotates through the bearings 74.
Four rows of shifting blocks 76 are uniformly arranged on the outer side wall of the pipe body 71 along the circumferential direction, and a plurality of non-row shifting blocks 76 are arranged; four rows of piezoelectric sheets 75 are vertically arranged on the inner wall of the tube body 71, the number of each row of piezoelectric sheets 75 is the same as that of the poking blocks 76, and when the tube body 71 rotates, the poking blocks 76 can interfere with the piezoelectric sheets 75; the plurality of piezoelectric sheets 75 are connected in series by wires, and a rectifier is connected to the piezoelectric sheets, and a display instrument is connected to the rectifier.
When the gas flow velocity detection unit 7 detects the gas, the mixed gas pressurized by the pressurization unit 6 quickly enters the pipe body 71, the inner diameter of the pipe body 71 is the same as the inner diameter of the pressurization member 68, after the gas flow enters the pipe body 71, the fan blade 72 arranged in the pipe body 71 is driven, the rotation of the fan blade 72 drives the pipe body 71 to rotate, when the pipe body 71 rotates, the poking block 76 arranged outside the pipe body 71 interferes with the piezoelectric sheet 75, the poking block 76 pokes the piezoelectric sheet 75 to vibrate, when the piezoelectric sheet 75 vibrates, the two ends of the piezoelectric sheet 75 generate a potential difference, the potential difference is connected with a rectifier through a lead to rectify the current to form a stable current, and the magnitude of the current is displayed through a connected display instrument, so that the magnitude of the current is in direct proportion to the flow velocity of the gas, the faster the flow velocity is, the rotation frequency of the pipe body 71 is faster, the larger the vibration amplitude and the higher frequency of the piezoelectric sheet 75 are, and the generated potential difference is larger and the larger current is; therefore, the flow velocity and the flow of the mixed gas flow can be directly reflected through the generated current, the reasonable setting of the molecular sieve in the separating mechanism 8 is convenient to control, the purpose of completely removing the water is achieved, and resources are reasonably allocated. In order to further improve the accuracy of the dosage of the molecular sieve and prevent the excessive waste of resources, the mass M1 of the molecular sieve and the gas flow velocity v2 after pressurization, the inner diameter r2 of the pressurization piece 68, the working time t and the mass M2 of the absorbed mixed gas water meet the conditions that M1= lambda.2 (v 2 pi r 2) 2 t)/M2•10 3 kg/m 3 (ii) a In the above formula, the unit of M1 and M2 is g, and λ is a relation adjusting coefficient, and the value range is 0.92-1.63. Meanwhile, in order to prevent the piezoelectric patch 75 from being broken in the using process, ensure the using stability of the piezoelectric patch, and increase the using fatigue, the thickness b of the piezoelectric patch 75, the length L of the piezoelectric patch 75, and the shore hardness thereofH and the rebound resilience k with the gas flow rate after pressurization v2, L/b = β (H-3 v 2) k; in the above formula, L, b has a unit of cm, beta is an adjusting coefficient, and the value range is 1.66-3.27.
Example four
As shown in fig. 7-9, the filtering mechanism 9 includes a housing 91, a fixed block 92 is connected to one side of the inside of the housing 91 close to the separating mechanism 8, a first spring 93 is connected to the other side of the fixed block 92, a moving plate 94 is connected to the other end of the first spring 93, and a trapezoidal block 95 is connected to the other side of the moving plate 94 close to the middle; a baffle 96 is arranged on one side of the moving plate 94 far away from the fixed block 92, the outer side of the baffle 96 is connected with the shell 91, the center position of the baffle 96 is of a hollow structure, and the moving plate 94 can be in sealing pressure connection with the baffle 96 through an arranged rubber ring.
Fixing boxes 97 are symmetrically arranged on two sides of one end, far away from the fixing block 92, in the shell 91, through grooves are formed in the side walls of the fixing boxes 97, guide rods 98 are arranged in the fixing boxes 97, sliding rings 99 are arranged on the guide rods 98, the sliding rings 99 are in sliding connection with the guide rods 98, the sliding rings 99 are connected with connecting rods 911, the connecting rods 911 are arranged in the through grooves, and the connecting rods 911 are in sliding connection with the through grooves; a spring is arranged on the guide rod 98, one end of the spring is connected with the sliding ring 99, and the other end of the spring is connected with the inner wall of the sealing box.
The other end of the connecting rod 911 is connected with a clamping block 912, the clamping block 912 is of a U-shaped structure, a filter body 913 is movably clamped on the clamping block 912, and a dilute hydrochloric acid solution is arranged inside the filter body 913; the housing 91 is provided with a movable door, and the filter 913 can be replaced by taking out the filter from the movable door.
When the filter mechanism 9 is to replace the filter body 913, when the filter body 913 is located in the buckle, the buckle is pressed against the baffle 96 to form a seal due to the elastic force of the second spring 910 applied to the slip ring 99 connected with the buckle, and at the same time, the filter body 913 presses the trapezoidal block 95, the trapezoidal block 95 pushes the moving plate 94 open, so that the moving plate 94 is separated from the baffle 96 to form a passage, and the exhaust gas on the left side of the filter body 913 can be filtered by the filter body 913 and discharged through the exhaust pipe 10; when the filter body 913 needs to be replaced, in order to prevent the filter body 913 from being drawn out, toxic methanol tail gas is directly discharged without being filtered, so that the environment is polluted and workers are harmed; when the filter 913 is drawn out, since the filter 913 is separated from the trapezoid block 95, the trapezoid block 95 is no longer under the pressure of the filter 913, the first spring 93 presses the moving plate 94 against the baffle 96 by the elastic force, and the baffle 96 and the moving plate 94 are tightly pressed by the rubber ring to form a closed circuit, so that when the filter 913 is drawn out, the tail gas containing a small amount of methanol which is not adsorbed is directly discharged from the tail gas pipe 10, thereby preventing air pollution and improving the safety of the equipment. In order to prevent the buckle from being separated from the baffle 96 during the insertion of the filter 913, and the gas is dispersed into the exhaust pipe 10 from the gap between the buckle and the baffle 96, so as to further increase the sealing performance, the elastic force F2 of the second spring 910 and the elastic force F1 of the first spring 93 satisfy: f2>2F1.
The device that obtains through above-mentioned technical scheme is a production technology of liquid sodium methoxide, through setting up the pressure boost unit, at the in-process of pressure boost, has not only improved the temperature of mist, makes its vaporization more abundant, becomes the molecular morphology, is favorable to subsequent abundant separation, and through the velocity of flow that improves mist moreover, helps carrying out the separation of methyl alcohol and vapor more high-efficiently, improves separation efficiency to further improve production efficiency. Through setting up air current velocity of flow detecting element, can direct reaction air current's velocity of flow and flow according to the electric current size that produces, the reasonable setting of the inside molecular sieve of the control separating mechanism of being convenient for reaches the purpose that moisture got rid of completely, and the rational allocation resource. Through setting up filtering mechanism, when the filtering body takes out, because filtering body and trapezoidal piece break away from, the trapezoidal piece no longer receives the pressure of filtering the body, and first spring passes through the effect of elasticity with movable plate crimping on the baffle to through the inseparable crimping of rubber ring between baffle and the movable plate, form the closed circuit, when preventing to extract the filtering body, the tail gas that contains a small amount of methyl alcohol is direct to be discharged from the tail gas pipe not adsorbing, prevents to cause air pollution, the security that lifting means used. The relationship between the stress area of the vertical axis wind wheel, the gas flow rate before pressurization, the gas flow rate after pressurization, the diameter of the gas outlet pipe and the inner diameter of the pressurization piece is limited, the pressurization effect is improved, the too large or too small stress area of the vertical axis wind wheel is prevented, and the piston plate is driven to reciprocate better. Through the relation between the mass of the molecular sieve and the gas flow rate after pressurization, the inner diameter of the pressurization piece, the working time and the mass of the absorbed mixed gas water, the accuracy of the using amount of the molecular sieve is further improved, and the excessive waste of resources is prevented. Through the thickness of injecing the piezoelectric patches, the length of piezoelectric patches and its shore hardness and the relation between the gas velocity of flow after the rebound ratio and the pressure boost, prevent the piezoelectric patches fracture in the use, guarantee its stability in use, increase and use fatigue.
Other technical solutions not described in detail in the present invention are prior art in the field, and are not described herein again.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art; any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. Step one, injecting a sodium hydroxide solution with the mass fraction of 22% and an anhydrous methanol solution into a tower body from a feed inlet, wherein the molar ratio of the methanol solution to the sodium hydroxide solution is 4.4, then starting an electric heater to heat the tower body, the heating temperature is 100-120 ℃, and starting a motor to stir;
step two, water generated in the reaction process is heated and evaporated into steam, the steam is discharged from an air outlet pipe at the top of the tower body along with the volatile gas of the methanol, then the steam is pressurized by a pressurizing unit, the temperature is raised and the steam is fully vaporized, the flow rate is detected by a gas flow rate detection unit, the flow rate of the gas is obtained according to the flow rate of the gas, and the consumption of the molecular sieve raw material in the separation mechanism is determined according to the flow rate of the mixed gas, so that the water molecules in the methanol are completely adsorbed and removed after passing through the separation mechanism, the methanol solution enters the tower body from a new return pipe for reaction, the water generated in the tower body is better removed, the reaction is promoted to be carried out in the direction of generating the sodium methoxide, the reverse reaction is prevented, and the purity of the obtained liquid sodium methoxide is improved;
and step three, the tail gas after passing through the separation mechanism enters a filtering mechanism, the filtering mechanism contains a filtering body provided with dilute hydrochloric acid, a small amount of methanol, sodium hydroxide and sodium methoxide contained in the tail gas can react through the filtering body containing the dilute hydrochloric acid, the tail gas pollution is reduced, an automatic sealing mechanism is arranged, when the filtering body is replaced, the sealing effect is automatically achieved, and the tail gas leakage and the environmental pollution caused by the replacement of the filtering body are prevented.
2. The production process of liquid sodium methoxide according to claim 1, wherein the production apparatus used in the production process comprises a tower body (1), the bottom of the tower body (1) is provided with a motor (2), an output shaft of the motor (2) penetrates through the bottom of the tower body (1), an output shaft of the motor (2) is connected with a stirrer (3), the stirrer (3) is connected with the tower body (1) in a sealing and rotating way, the side wall of the tower body (1) is provided with an electric heater (4), the top of the tower body (1) is connected with an air outlet pipe (5), one end of the air outlet pipe (5) close to the tower body (1) is provided with a pressurizing unit (6), the pressurizing unit (6) pressurizes the gas in the air outlet pipe (5), the other end of the pressurizing unit (6) is provided with a gas flow velocity detection unit (7), the gas flow velocity detection unit (7) is arranged inside the gas outlet pipe (5), the other end of the air outlet pipe (5) is connected with the upper end of the separating mechanism (8), the bottom of the separating mechanism (8) is connected with a return pipe (13), the other end of the return pipe (13) is communicated with the tower body (1), the side wall of the separation mechanism (8) close to the bottom is connected with a filtering mechanism (9), the other end of the filtering mechanism (9) is connected with a tail gas pipe (10); the tower body (1) is equipped with feed inlet (11) near the position at top, and tower body (1) is equipped with discharge gate (12) near the position of bottom.
3. The production process of liquid sodium methoxide according to claim 2, wherein the pressurization mechanism comprises a vertical axis wind wheel (61), the vertical axis wind wheel (61) is disposed inside the air outlet pipe (5), two sides of the vertical axis wind wheel (61) are both provided with rotating shafts, the rotating shafts penetrate through the wall of the air outlet pipe (5), the rotating shafts are hermetically and rotatably connected with the wall of the air outlet pipe (5), the rotating shafts on two sides of the vertical axis wind wheel (61) are both linked with a cam (62), the other side of the cam (62) is rotatably connected with a connecting rod (63), and the other end of the connecting rod (63) is rotatably connected with a telescopic rod (64); the two sides of the air outlet pipe (5) are respectively provided with a sealing box body (65), the other end of the telescopic rod (64) extends into the sealing box body (65), the telescopic rod (64) is in sealing sliding connection with the sealing box body (65) through an arranged rubber pad, and the other end of the telescopic rod (64) is connected with a piston plate (66); one side of the sealing box body (65) far away from the telescopic rod (64) is provided with an increasing piece, the center of the increasing piece (68) is provided with a round hole, the diameter of the air outlet pipe (5) is reduced, one side of the sealing box body (65) far away from the air outlet pipe (5) is connected with an air guide pipe (67), and the other end of the air guide pipe (67) is communicated with the pressurizing piece (68).
4. The production process of liquid sodium methoxide according to claim 3, wherein a partition plate (613) is disposed inside the sealed box (65), the piston plate (66) and the outer sidewall of the gas outlet pipe (5) are in sealed sliding contact with the partition plate (613), and the gas outlet pipe (5) has a rectangular parallelepiped structure; one end, close to the vertical shaft wind wheel (61), of the air outlet pipe (5) positioned in the sealed box body (65) is provided with a first air inlet 69, one end, close to the pressurizing piece (68), is provided with a second air inlet 610, one side, close to the vertical shaft wind wheel (61), of the partition plate (613) is provided with a first air outlet 611, and one side, close to the pressurizing piece, of the partition plate (613) is provided with a second air outlet 612; the first air inlet 69 and the second air inlet 610 are both provided with inlet valves, the inlet valves are rotatably connected with the outer side wall of the air outlet pipe (5) through hinges, the first air outlet 611 and the second air outlet 612 are both provided with air outlet valves, and the air outlet valves are rotatably connected with one side, away from the piston plate (66), of the partition plate (613) through hinges.
5. The production process of liquid sodium methoxide according to claim 2, wherein the gas flow rate detection unit (7) comprises a pipe body (71), the pipe body (71) is disposed inside the gas outlet pipe (5), fan blades (72) are disposed inside the pipe body (71), bearings (74) are disposed at two ends of the pipe body (71), a support rod (73) is connected to the outer side of each bearing (74), the other end of each support rod (73) is connected to the inner side wall of the gas outlet pipe (5), and the pipe body (71) rotates through the disposed bearings (74).
6. The production process of liquid sodium methoxide according to claim 5, wherein four rows of stirring blocks (76) are uniformly arranged on the outer side wall of the pipe body (71) along the circumferential direction, and a plurality of stirring blocks (76) are arranged; four rows of piezoelectric sheets (75) are vertically arranged on the inner wall of the tube body (71), the number of each row of piezoelectric sheets (75) is the same as that of the poking blocks (76), and when the tube body (71) rotates, the poking blocks (76) can interfere with the piezoelectric sheets (75); the piezoelectric sheets (75) are connected in series through wires, and are connected with a rectifier, and the display instrument is connected with the rectifier.
7. The production process of liquid sodium methoxide according to claim 2, characterized in that the filtering mechanism (9) comprises a housing (91), one side of the interior of the housing (91) close to the separating mechanism (8) is connected with a fixed block (92), the other side of the fixed block (92) is connected with a first spring (93), the other end of the first spring (93) is connected with a moving plate (94), and the other side of the moving plate (94) close to the middle position is connected with a trapezoidal block (95); one side of the moving plate (94) far away from the fixed block (92) is provided with a baffle (96), the outer side of the baffle (96) is connected with the shell (91), the center position of the baffle (96) is of a hollow structure, and the moving plate (94) can be in sealing pressure connection with the baffle (96) through a rubber ring.
8. The production process of liquid sodium methoxide according to claim 7, wherein fixing boxes (97) are symmetrically arranged at two sides of one end of the interior of the shell (91) far away from the fixing block (92), through grooves are formed in the side walls of the fixing boxes (97), guide rods (98) are arranged in the fixing boxes (97), sliding rings (99) are arranged on the guide rods (98), the sliding rings (99) are slidably connected with the guide rods (98), the sliding rings (99) are connected with connecting rods (911), the connecting rods (911) are arranged in the through grooves, and the connecting rods (911) are slidably connected with the through grooves; and a spring is arranged on the guide rod (98), one end of the spring is connected with the sliding ring (99), and the other end of the spring is connected with the inner wall of the sealing box.
9. The production process of liquid sodium methoxide according to claim 8, wherein a clamping block (912) is connected to the other end of the connecting rod (911), the clamping block (912) is of a U-shaped structure, a filter body (913) is movably clamped on the clamping block (912), and a dilute hydrochloric acid solution is arranged inside the filter body (913); the shell (91) is provided with a movable door, and the filter body (913) can be taken out of the movable door for replacement.
10. The production process of liquid sodium methoxide according to claim 2, wherein multiple layers of molecular sieves are arranged in the separation mechanism (8), and the molecular sieves are 3A molecular sieves consisting of sodium aluminosilicate or sodium calcium aluminosilicate.
CN202211481106.9A 2022-11-24 2022-11-24 Production process of liquid sodium methoxide Pending CN115745743A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116808949A (en) * 2023-08-29 2023-09-29 昆明贵金属研究所 Continuous reaction device for preparing formic acid by carbon dioxide hydrogenation

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1626488A (en) * 2004-08-13 2005-06-15 于志波 Technique of alkaline process for producing sodium methoxide/sodium ethylate
CN112209808A (en) * 2020-09-15 2021-01-12 安徽金邦医药化工有限公司 Novel process for producing sodium methoxide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1626488A (en) * 2004-08-13 2005-06-15 于志波 Technique of alkaline process for producing sodium methoxide/sodium ethylate
CN112209808A (en) * 2020-09-15 2021-01-12 安徽金邦医药化工有限公司 Novel process for producing sodium methoxide

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116808949A (en) * 2023-08-29 2023-09-29 昆明贵金属研究所 Continuous reaction device for preparing formic acid by carbon dioxide hydrogenation
CN116808949B (en) * 2023-08-29 2023-11-03 昆明贵金属研究所 Continuous reaction device for preparing formic acid by carbon dioxide hydrogenation

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