CN212347747U - Methyl phosphine aldehyde reaction liquid continuous evaporation and concentration device - Google Patents
Methyl phosphine aldehyde reaction liquid continuous evaporation and concentration device Download PDFInfo
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- CN212347747U CN212347747U CN202020874228.4U CN202020874228U CN212347747U CN 212347747 U CN212347747 U CN 212347747U CN 202020874228 U CN202020874228 U CN 202020874228U CN 212347747 U CN212347747 U CN 212347747U
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Abstract
The invention discloses a continuous evaporation and concentration device for methyl phosphine aldehyde reaction liquid, which comprises a reaction liquid storage tank, a conveying pump, a film evaporator, a 1# methyl phosphine aldehyde storage tank, a 2# methyl phosphine aldehyde storage tank, a gas condensation and collection device and a vacuum pump, wherein the vacuum in the film evaporator is maintained under the operation action of the vacuum pump, the 1# methyl phosphine aldehyde storage tank and the 2# methyl phosphine aldehyde storage tank are mutually standby, and when one is in a liquid storage state, the other is used for discharging liquid. The device can realize high-efficiency continuous evaporation of the solvent in the methyl phosphine aldehyde reaction liquid under the low-temperature condition, is simple in process, uniform in film distribution in the film evaporator, high in evaporation speed, short in reaction liquid retention time, low in energy consumption, capable of greatly improving the treatment capacity of the methyl phosphine aldehyde reaction liquid, and convenient to clean.
Description
Technical Field
The invention relates to a continuous evaporation and concentration device for methyl phosphine aldehyde reaction liquid.
Background
Glufosinate is a novel green and environment-friendly herbicide and is an ideal agent for replacing glyphosate. Methyl phosphine aldehyde is a key intermediate product in the production process of glufosinate-ammonium, the distillation separation process of a solvent in the existing methyl phosphine aldehyde reaction liquid is usually carried out in a reaction kettle, and the process is an intermittent operation process, so that the defects of low purity of intermediate products, high energy consumption, poor separation effect, high equipment investment, large occupied area and the like exist, the production and popularization of glufosinate-ammonium products are severely limited, the components of a gas-phase condensed recovery liquid are complex, and the recovery cost of the solvent is greatly increased.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a continuous evaporation and concentration device for a methyl phosphine aldehyde reaction solution, which solves the defects of low separation efficiency, high energy consumption, poor separation effect and the like in the distillation and separation process of the existing methyl phosphine aldehyde reaction solution, effectively improves the purity of a methyl phosphine aldehyde intermediate product, and reduces the recovery cost of a solvent.
The continuous evaporation and concentration device for the methyl phosphine aldehyde reaction liquid is characterized in that: the device comprises a thin film evaporator, wherein a liquid inlet at the upper part of the thin film evaporator is sequentially connected with a conveying pump and a reaction liquid storage tank through pipelines, a stirrer for stirring liquid in the thin film evaporator is arranged at the top of the thin film evaporator, a gas outlet at the upper part of the thin film evaporator is sequentially connected with a gas condensation and collection device and a vacuum pump through pipelines, the vacuum state in the thin film evaporator is maintained under the operation action of the vacuum pump, and the gas condensation and collection device is used for condensing and collecting a gas-phase solvent flowing out of a gas outlet at the upper part of; a liquid outlet at the bottom of the thin film evaporator is divided into two paths, one path is connected with a 1# methylphosphinic aldehyde storage tank through a 1# liquid phase outlet pipeline, and the other path is connected with a 2# methylphosphinic aldehyde storage tank through a 2# liquid phase outlet pipeline; the liquid level meter comprises a 1# liquid phase outlet pipeline, a 2# liquid phase outlet pipeline, a 1# liquid level meter, a 2# liquid level meter and a PLC control system, wherein the 1# liquid phase outlet pipeline and the 2# liquid phase outlet pipeline are respectively provided with the 1# electromagnetic valve and the 2# electromagnetic valve;
when the 1# liquid level meter measures that the liquid level in the 1# methylphosphine aldehyde storage tank reaches a set liquid level, transmitting a liquid level signal to the PLC control system, and feeding back and controlling the 1# electromagnetic valve to be closed and the 2# electromagnetic valve to be opened through the PLC control system; when the 2# liquid level meter measures that the liquid level in the 2# methylphosphine aldehyde storage tank reaches a set liquid level, transmitting a liquid level signal to the PLC control system, feeding back and controlling the 2# electromagnetic valve to be closed and the 1# electromagnetic valve to be opened through the PLC control system, so that the 1# methylphosphine aldehyde storage tank and the 2# methylphosphine aldehyde storage tank are mutually standby, and when one is in a liquid storage state, the other is discharged, thereby realizing the continuous evaporation of the methylphosphine aldehyde reaction liquid; control valves are arranged on the corresponding pipelines.
The continuous evaporation and concentration device for the methyl phosphine aldehyde reaction liquid is characterized in that: the gas condensation and collection device comprises a primary gas phase condenser, a No. 1 concentrated solution receiving tank and a secondary gas phase condenser, wherein the primary gas phase condenser and the secondary gas phase condenser are both in heat exchanger structures, a gas outlet at the upper part of the thin film evaporator is connected with an inlet of the primary gas phase condenser through a gas phase outlet pipeline, a gas phase outlet at the upper part of the primary gas phase condenser is connected with the secondary gas phase condenser through a non-condensable gas outlet pipeline, and a gas phase outlet at the upper part of the secondary gas phase condenser is connected with a vacuum pump through;
the liquid phase outlet at the bottom of the secondary gas phase condenser is connected with the primary condensate outlet pipeline through the secondary condensate outlet pipeline so as to collect the condensed solvent concentrated solution of the primary gas phase condenser and the condensed solvent concentrated solution of the secondary gas phase condenser into the 1# concentrated solution receiving tank respectively.
The continuous evaporation and concentration device for the methyl phosphine aldehyde reaction liquid is characterized in that: the device also comprises a No. 2 concentrated solution receiving tank, wherein a liquid inlet at the top of the No. 2 concentrated solution receiving tank is connected with a primary condensate outlet pipeline through a condensate inlet pipeline; a 3# electromagnetic valve is arranged on a primary condensate outlet pipeline between the condensate inlet pipeline and the 1# concentrated solution receiving tank, a 4# electromagnetic valve is arranged on the condensate inlet pipeline, a 3# liquid level meter and a 4# liquid level meter are respectively arranged on the 1# concentrated solution receiving tank and the 2# concentrated solution receiving tank, and the 3# liquid level meter and the 4# liquid level meter are simultaneously in signal connection with the 3# electromagnetic valve and the 4# electromagnetic valve through a PLC control system;
when the 3# liquid level meter measures that the liquid level in the 1# concentrated liquid receiving tank reaches a set liquid level, a liquid level signal is transmitted to the PLC control system, and the 3# electromagnetic valve is fed back and controlled to be closed and the 4# electromagnetic valve is controlled to be opened through the PLC control system; when the No. 4 liquid level meter measures that the liquid level in the No. 2 concentrated solution receiving groove reaches a set liquid level, a liquid level signal is transmitted to the PLC control system, the PLC control system feeds back and controls the No. 4 electromagnetic valve to be closed and the No. 3 electromagnetic valve to be opened, so that the No. 1 concentrated solution receiving groove and the No. 2 concentrated solution receiving groove are mutually standby, when one is in a liquid storage state, the other is used for discharging liquid, and therefore continuous evaporation of the methyl phosphine aldehyde reaction liquid is achieved;
the liquid outlets at the bottoms of the 1# concentrated solution receiving tank and the 2# concentrated solution receiving tank are connected with a condensate recovery pipeline through a branch pipe provided with a control valve, and the concentrated solution of the solvent collected in the 1# concentrated solution receiving tank or the 2# concentrated solution receiving tank is sent to a solvent recovery system through the condensate recovery pipeline for refining and recycling.
The continuous evaporation and concentration device for the methyl phosphine aldehyde reaction liquid is characterized in that: the primary gas-phase condenser and the secondary gas-phase condenser are both of heat exchanger structures, a primary condensing medium inlet pipeline and a primary condensing medium outlet pipeline are respectively connected to an inlet and an outlet of a cold channel of the primary gas-phase condenser through an inlet and an outlet, a secondary condensing medium inlet pipeline and a secondary condensing medium outlet pipeline are respectively connected to an inlet and an outlet of a cold channel of the secondary gas-phase condenser through an inlet and an outlet, and condensing media are respectively introduced into the cold channel of the primary gas-phase condenser and the cold channel of the secondary gas-phase; the vacuum pump inlet pipeline is connected with a nitrogen inlet pipeline, the top of the No. 1 concentrated solution receiving tank is connected with the vacuum pump inlet pipeline through a gas phase balance pipeline, and the top of the No. 2 concentrated solution receiving tank is connected with the gas phase balance pipeline through a branch pipe.
The continuous evaporation and concentration device for the methyl phosphine aldehyde reaction liquid is characterized in that: the reaction liquid storage tank is vertical, is made of PO (stainless steel) lined with steel, carbon steel or stainless steel, and has a volume of 5-30 m3To (c) to (d); the device comprises a conveying pump shielding pump, a pneumatic diaphragm pump or a metering pump, wherein an outlet of the conveying pump is connected with a liquid inlet in the upper part of the thin film evaporator through an outlet pipeline of the conveying pump, a flow meter and a control valve are arranged on the outlet pipeline of the conveying pump, and the flow of methyl phosphine aldehyde reaction liquid conveyed into the thin film evaporator is controlled to be 1-5 m3/h；
The No. 1 methyl phosphine aldehyde storage tank or the No. 2 methyl phosphine aldehyde storage tank is made of PO lined with steel, carbon steel, stainless steel or glass lining, and has a volume of 5-30 m3In the meantime.
The continuous evaporation and concentration device for the methyl phosphine aldehyde reaction liquid is characterized in that: the thin film evaporator is provided with a thermometer for measuring the temperature of liquid inside the thin film evaporator, the side part of the thin film evaporator is sleeved with a heat exchange jacket, an inlet and an outlet of the heat exchange jacket are respectively communicated with a heating medium inlet pipeline and a heating medium outlet pipeline, the heating medium introduced into the heat exchange jacket is high-temperature steam or hot water, and the heat exchange area of the heat exchange jacket is 2-20 m2(ii) a The heating medium inlet pipeline is provided with a No. 5 electromagnetic valve, the No. 5 electromagnetic valve is in signal connection with a thermometer on the thin film evaporator through a PLC control system, the thermometer transmits the measured liquid temperature to the PLC control system, and the opening size of the No. 5 electromagnetic valve is fed back and controlled through the PLC control system so as to adjust and control the liquid phase temperature in the thin film evaporator.
Said oneA methyl phosphine aldehyde reaction liquid continuous evaporation concentration device is characterized in that: the condensing medium introduced into the cold channel of the first-stage gas phase condenser is circulating water, low-temperature water or frozen brine, and the heat exchange area of the condensing medium is 10-50 m2(ii) a The condensing medium introduced into the cold channel of the two-stage gas phase condenser is low-temperature water or frozen brine, and the heat exchange area of the condensing medium is 5-40 m2(ii) a The No. 1 concentrated solution receiving tank or the No. 2 concentrated solution receiving tank is made of PO lined with steel, carbon steel or stainless steel, and has a volume of 5-30 m3In the meantime.
A continuous evaporation and concentration process of methyl phosphine aldehyde reaction liquid is characterized by comprising the following steps:
step S1 evaporation preheating: starting a vacuum pump to enable the pressure in the methyl phosphine aldehyde reaction liquid continuous evaporation concentration device to be in a negative pressure state, starting a stirrer at the top of the thin film evaporator to stir, opening a heating medium inlet pipeline and a heating medium outlet pipeline on a heat exchange jacket at the side part of the thin film evaporator, setting the evaporation temperature of liquid in the thin film evaporator, and controlling the temperature of the liquid in the thin film evaporator to be maintained at the set temperature through interlocking of a No. 5 electromagnetic valve and a signal of a thermometer on the thin film evaporator;
step S2 feed control: conveying the methyl phosphine aldehyde reaction liquid in the reaction liquid storage tank into a thin film evaporator through a conveying pump, and controlling the feeding flow of the methyl phosphine aldehyde reaction liquid by adjusting a control valve and a flow meter on an outlet pipeline of the conveying pump;
step S3 thin film evaporation: the method comprises the following steps that (1) methyl phosphine aldehyde reaction liquid enters a film evaporator to centrifugally rotate at a high speed under the driving of a conveying pump, is in contact with the inner wall of the film evaporator and exchanges heat with a heating medium in a heat exchange jacket at the side part of the film evaporator to separate a solvent in the methyl phosphine aldehyde reaction liquid from methyl phosphine aldehyde, wherein the bottom of the methyl phosphine aldehyde is liquid-phase methyl phosphine aldehyde, the methyl phosphine aldehyde enters a 1# methyl phosphine aldehyde storage tank or a 2# methyl phosphine aldehyde storage tank, the upper part of the methyl phosphine aldehyde reaction liquid is vaporized solvent gas, and a gas phase condensation process is performed;
step S4 gas phase condensation: the gas phase at the upper part of the thin film evaporator enters a first-stage gas phase condenser through a gas phase outlet pipeline connected with a gas outlet at the upper part of the thin film evaporator for primary condensation, the non-condensable gas flowing out of a gas phase outlet at the upper part of the first-stage gas phase condenser enters a second-stage gas phase condenser through a non-condensable gas outlet pipeline for deep condensation, a gas phase outlet at the upper part of the second-stage gas phase condenser is connected with a vacuum pump through a pipeline, the solvent concentrated solution condensed by the first-stage gas phase condenser and the second-stage gas phase condenser enters a No. 1 concentrated solution receiving tank or a No. 2 concentrated solution receiving tank together for storage, and then the;
step S5 vacuum displacement: after evaporation and concentration are finished, closing a vacuum pump and a stirrer of the thin film evaporator, closing valves of a heating medium inlet pipeline and a heating medium outlet pipeline, opening a nitrogen inlet pipeline to fill nitrogen into the whole device for gas replacement, closing the nitrogen inlet pipeline after the pressure in the methyl phosphine aldehyde reaction liquid continuous evaporation and concentration device is normal pressure, starting the vacuum pump to pump negative pressure, opening the nitrogen inlet pipeline for gas replacement after evacuation is finished, and finally enabling the whole device to be in a nitrogen protection state.
The components of the methyl phosphine aldehyde reaction solution comprise, by weight, 40-80% of methyl phosphine aldehyde, 10-50% of ethanol and 10-30% of water; the vacuum degree in the film evaporator is-0.05 Kpa-50 Kpa, the temperature of a gas phase outlet at the upper part of the first-stage gas phase condenser is controlled to be 40-60 ℃, and the temperature of a gas phase outlet at the upper part of the second-stage gas phase condenser is controlled to be 15-25 ℃.
The beneficial effect that this application was got is: the continuous evaporation and concentration device for the methyl phosphine aldehyde reaction liquid can effectively overcome the defects of low separation efficiency, high energy consumption, poor separation effect and the like in the distillation and separation process of the methyl phosphine aldehyde reaction liquid, improve the purity of an intermediate product and reduce the recovery cost of a solvent. The device can realize high-efficiency continuous evaporation of the solvent in the methyl phosphine aldehyde reaction liquid under the low-temperature condition, is simple in process, uniform in film distribution in the film evaporator, high in evaporation speed, short in reaction liquid retention time, low in energy consumption, capable of greatly improving the treatment capacity of the methyl phosphine aldehyde reaction liquid, and convenient to clean.
Drawings
FIG. 1 is a schematic structural diagram of a methyl phosphine aldehyde reaction liquid continuous evaporation and concentration device according to the present invention;
in fig. 1: a reaction liquid storage tank; 2-a delivery pump; 3-a thin film evaporator; a 4-1# methylphosphinic aldehyde storage tank; a 5-2# methylphosphinic aldehyde storage tank; 6-first-stage gas phase condenser; 7-a secondary gas phase condenser; a 8-1# concentrated solution receiving tank; a 9-2# concentrated solution receiving tank and a 10-vacuum pump; an outlet pipeline of the 101-methyl phosphine aldehyde reaction liquid; 102-a transfer pump outlet conduit; 103-1# liquid phase outlet pipeline; 104-2# liquid phase outlet conduit; 105-a gas phase outlet conduit; 106-noncondensable gas outlet conduit; 107-primary condensate outlet conduit; 108-secondary condensate outlet conduit; 109-condensate inlet conduit; 110-vacuum pump inlet line; 111-nitrogen inlet line; 112-gas phase equilibrium conduit; 113-heating medium inlet conduit; 114-heating medium outlet conduit; 115-primary condensing medium inlet conduit; 116-a primary condensing medium outlet conduit; 117-secondary condensing medium inlet conduit; 118-secondary condensing medium outlet conduit; 119-condensate recovery line.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b): compare FIG. 1
A methyl phosphine aldehyde reaction liquid continuous evaporation and concentration device comprises a reaction liquid storage tank 1, a delivery pump 2, a thin film evaporator 3, a 1# methyl phosphine aldehyde storage tank 4, a 2# methyl phosphine aldehyde storage tank 5, a primary gas phase condenser 6, a secondary gas phase condenser 7, a 1# concentrated liquid receiving tank 8, a 2# concentrated liquid receiving tank 9 and a vacuum pump 10.
The reaction liquid storage tank 1 is internally filled with methyl phosphine aldehyde reaction liquid, the reaction liquid storage tank 1 is connected with an inlet of the conveying pump 2 through a methyl phosphine aldehyde reaction liquid outlet pipeline 101, and an outlet of the conveying pump 2 is connected with a liquid inlet at the upper part of the thin film evaporator 3 through a conveying pump outlet pipeline 102. The top of the thin film evaporator 3 is provided with a stirrer for stirring liquid in the thin film evaporator, a gas outlet at the upper part of the thin film evaporator 3 is sequentially connected with a gas condensation and collection device and a vacuum pump 10 through pipelines, the vacuum state in the thin film evaporator 3 is maintained under the operation action of the vacuum pump 10, and the gas condensation and collection device is used for condensing and collecting a gas-phase solvent flowing out of the gas outlet at the upper part of the thin film evaporator 3.
Wherein, the gas condensation collection device comprises a first-stage gas phase condenser 6, a 1# concentrated solution receiving groove 8, a second-stage gas phase condenser 7 and a 2# concentrated solution receiving groove 9. As can be seen from the comparison of fig. 1, the first-stage gas phase condenser 6 and the second-stage gas phase condenser 7 are both heat exchanger structures, the inlet and outlet of the cold channel of the first-stage gas phase condenser 6 are respectively connected with a first-stage condensing medium inlet pipeline 115 and a first-stage condensing medium outlet pipeline 116, the inlet and outlet of the cold channel of the second-stage gas phase condenser 7 are respectively connected with a second-stage condensing medium inlet pipeline 117 and a second-stage condensing medium outlet pipeline 118, and condensing mediums are respectively introduced into the cold channel of the first-stage gas phase condenser 6 and the cold channel of the.
The liquid phase outlet at the bottom of the heat channel of the first-stage gas phase condenser 6 is connected with the 1# concentrated solution receiving tank 8 through a first-stage condensate outlet pipeline 107, and the liquid phase outlet at the bottom of the heat channel of the second-stage gas phase condenser 7 is connected with the first-stage condensate outlet pipeline 107 through a second-stage condensate outlet pipeline 108, so that the solvent concentrated solutions condensed by the first-stage gas phase condenser 6 and the second-stage gas phase condenser 7 are respectively collected into the 1# concentrated solution receiving tank 8. The liquid inlet at the top of the 2# concentrated solution receiving groove 9 is connected with a primary condensate outlet pipeline 107 through a condensate inlet pipeline 109, so that the solvent concentrated solution condensed by the primary gas-phase condenser 6 and the secondary gas-phase condenser 7 can be collected in the 2# concentrated solution receiving groove 9.
No. 1 concentrate receiving tank 8 and No. 2 concentrate receiving tank 9 are each other spare-minded, and the concrete process is: be equipped with the 3# solenoid valve on the one-level condensate outlet pipe 107 between condensate inlet pipe 109 and the 1# concentrate receiving groove 8, be equipped with the 4# solenoid valve on the condensate inlet pipe 109, be equipped with 3# level gauge and 4# level gauge on 1# concentrate receiving groove 8 and the 2# concentrate receiving groove 9 respectively, 3# level gauge and 4# level gauge all through PLC control system simultaneously with 3# solenoid valve and 4# solenoid valve signal connection. When the 3# liquid level meter measures that the liquid level in the 1# concentrated liquid receiving groove 8 reaches a set liquid level, a liquid level signal is transmitted to the PLC control system, and the 3# electromagnetic valve is fed back and controlled to be closed and the 4# electromagnetic valve is controlled to be opened through the PLC control system; when the liquid level that 4# level gauge measured in 2# concentrate receiving groove 9 reached the settlement liquid level, give PLC control system with liquid level signal transmission, through PLC control system feedback and control 4# solenoid valve and close and 3# solenoid valve is opened, from this 1# concentrate receiving groove 8 and 2# concentrate receiving groove 9 are each other for reserve, and when one was in stock solution state, another was put the liquid to realize methyl phosphine aldehyde reaction liquid continuous evaporation.
The liquid outlets at the bottoms of the 1# concentrated solution receiving tank 8 and the 2# concentrated solution receiving tank 9 are connected with a condensate recovery pipeline 119 through a branch pipe provided with a control valve, and the concentrated solution of the solvent collected in the 1# concentrated solution receiving tank 8 or the 2# concentrated solution receiving tank 9 is sent to a solvent recovery system through the condensate recovery pipeline 119 for refining and recycling.
The gas outlet at the upper part of the thin film evaporator 3 is connected with the inlet of the hot channel of the first-stage gas phase condenser 6 through a gas outlet pipeline 105, the gas outlet at the upper part of the hot channel of the first-stage gas phase condenser 6 is connected with the inlet of the hot channel of the second-stage gas phase condenser 7 through a non-condensable gas outlet pipeline 106, and the gas outlet at the upper part of the hot channel of the second-stage gas phase condenser 7 is connected with the vacuum pump 10 through a vacuum. The vacuum pump inlet pipeline 110 is connected with a nitrogen inlet pipeline 111, the top of the No. 1 concentrated solution receiving tank 8 is connected with the vacuum pump inlet pipeline 110 through a gas phase balance pipeline 112, and the top of the No. 2 concentrated solution receiving tank 9 is connected with the gas phase balance pipeline 112 through a branch pipe.
The liquid outlet at the bottom of the hot channel of the film evaporator 3 is divided into two paths, one path is connected with a 1# methylphosphinic aldehyde storage tank 4 through a 1# liquid phase outlet pipeline 103, and the other path is connected with a 2# methylphosphinic aldehyde storage tank 5 through a 2# liquid phase outlet pipeline 104; wherein be equipped with 1# solenoid valve and 2# solenoid valve on 1# liquid phase outlet pipeline 103 and the 2# liquid phase outlet pipeline 104 respectively, be equipped with 1# level gauge and 2# level gauge on 1# methyl phosphine aldehyde storage tank 4 and the 2# methyl phosphine aldehyde storage tank 5 respectively, 1# level gauge and 2# level gauge all through PLC control system simultaneously with 1# solenoid valve and 2# solenoid valve signal connection. When the 1# liquid level meter measures that the liquid level in the 1# methylphosphine aldehyde storage tank 4 reaches a set liquid level, transmitting a liquid level signal to the PLC control system, and feeding back and controlling the 1# electromagnetic valve to be closed and the 2# electromagnetic valve to be opened through the PLC control system; when the 2# liquid level meter measures that the liquid level in the 2# methyl phosphine aldehyde storage tank 5 reaches a set liquid level, a liquid level signal is transmitted to the PLC control system, the 2# electromagnetic valve is controlled to be closed and the 1# electromagnetic valve is controlled to be opened through feedback of the PLC control system, therefore, the 1# methyl phosphine aldehyde storage tank 4 and the 2# methyl phosphine aldehyde storage tank 5 are mutually standby, when one is in a liquid storage state, the other is discharged, and therefore continuous evaporation of methyl phosphine aldehyde reaction liquid is achieved; control valves are arranged on the corresponding pipelines.
The reaction liquid storage tank 1 is vertical, is made of steel lining PO, carbon steel, stainless steel and the like, and has a volume of 5-30 m3In the meantime.
The material of the conveying pump 2 is steel lining PTFE and the like, the outlet of the conveying pump 2 is connected with the liquid inlet at the upper part of the thin film evaporator 3 through an outlet pipeline 102, the outlet pipeline 102 of the conveying pump is provided with a flowmeter and a control valve, and the flow of the methyl phosphine aldehyde reaction liquid conveyed into the thin film evaporator 3 is controlled to be 1-5 m3/h。
The No. 1 methyl phosphine aldehyde storage tank 4 or the No. 2 methyl phosphine aldehyde storage tank 5 is made of PO lined with steel, carbon steel, stainless steel or glass lining, and has a volume of 5-30 m3In the meantime.
The condensing medium introduced into the cold channel of the first-stage gas phase condenser 6 is circulating water, low-temperature water or frozen brine, and the heat exchange area of the condensing medium is 10-50 m2(ii) a The condensing medium introduced into the cold channel of the secondary gas phase condenser 7 is low-temperature water or frozen brine, and the heat exchange area of the condensing medium is 5-40 m2(ii) a The No. 1 concentrated solution receiving tank 8 or the No. 2 concentrated solution receiving tank 9 is made of PO lined with steel, carbon steel or stainless steel, and has a volume of 5-30 m3In the meantime.
The vacuum pump 10 is a water ring vacuum pump, a Roots reciprocating vacuum unit and the like.
The thin film evaporator 3 is provided with a thermometer for measuring the temperature of liquid inside the thin film evaporator 3, the side part of the thin film evaporator 3 is sleeved with a heat exchange jacket, the inlet and the outlet of the heat exchange jacket are respectively communicated with a heating medium inlet pipeline 113 and a heating medium outlet pipeline 114, the heating medium introduced into the heat exchange jacket is high-temperature steam or hot water, and the heat exchange area of the heat exchange jacket is 2-20 m2(ii) a A 5# electromagnetic valve is arranged on the heating medium inlet pipeline 113, the 5# electromagnetic valve is in signal connection with a thermometer on the film evaporator 3 through a PLC control system, and the thermometer transmits the measured liquid temperatureAnd feeding back and controlling the opening of the 5# electromagnetic valve through the PLC control system so as to regulate and control the liquid phase temperature in the thin film evaporator 3.
The invention relates to a continuous evaporation and concentration process of methyl phosphine aldehyde reaction liquid, which comprises the following steps:
step S1 evaporation preheating: starting a vacuum pump 10 to enable the pressure in the methyl phosphine aldehyde reaction liquid continuous evaporation and concentration device to be in a negative pressure state, starting a stirrer at the top of the thin film evaporator 3 to stir, opening a heating medium inlet pipeline 113 and a heating medium outlet pipeline 114 on a heat exchange jacket at the side part of the thin film evaporator 3, setting the evaporation temperature of the liquid in the thin film evaporator 3, and controlling the temperature of the liquid in the thin film evaporator 3 to be maintained at the set temperature through signal interlocking of a No. 5 electromagnetic valve and a thermometer on the thin film evaporator 3 (namely the No. 5 electromagnetic valve is in signal connection with the thermometer on the thin film evaporator 3 through a PLC control system);
step S2 feed control: the methyl phosphine aldehyde reaction liquid in the reaction liquid storage tank 1 is conveyed into a thin film evaporator 3 through a conveying pump 2, and the feeding flow of the methyl phosphine aldehyde reaction liquid is controlled by adjusting a control valve and a flow meter on an outlet pipeline 102 of the conveying pump;
step S3 thin film evaporation: the method comprises the following steps of (1) enabling methyl phosphine aldehyde reaction liquid to enter a thin film evaporator 3 to centrifugally rotate at a high speed under the driving of a conveying pump 2, enabling the methyl phosphine aldehyde reaction liquid to be in contact with the inner wall of the thin film evaporator 3 and to exchange heat with a heating medium in a heat exchange jacket on the side part of the thin film evaporator 3, enabling a solvent in the methyl phosphine aldehyde reaction liquid to be separated from methyl phosphine aldehyde, enabling the methyl phosphine aldehyde with a liquid phase at the bottom to enter a 1# methyl phosphine aldehyde storage tank 4 or a 2# methyl phosphine aldehyde storage tank 5, enabling vaporized solvent gas to be at the upper part, and performing a gas phase removing;
step S4 gas phase condensation: the gas phase on the upper part of the thin film evaporator 3 enters a first-stage gas phase condenser 6 for primary condensation through a gas phase outlet pipeline 105 connected with a gas outlet on the upper part of the thin film evaporator 3, non-condensable gas flowing out of a gas phase outlet on the upper part of the first-stage gas phase condenser 6 enters a second-stage gas phase condenser 7 for deep condensation through a non-condensable gas outlet pipeline 106, the gas phase outlet on the upper part of the second-stage gas phase condenser 7 is connected with a vacuum pump 10 through a pipeline, solvent concentrated solution condensed by the first-stage gas phase condenser 6 and the second-stage gas phase condenser 7 enters a No. 1 concentrated solution receiving tank 8 or a No. 2 concentrated solution receiving tank (9) for storage, and then the solvent concentrated solution is;
step S5 vacuum displacement: after evaporation and concentration are finished, the vacuum pump 10 and the stirrer of the thin film evaporator 3 are closed, valves of a heating medium inlet pipeline 113 and a heating medium outlet pipeline 114 are closed, a nitrogen inlet pipeline 111 is opened to fill nitrogen into the whole device for gas replacement, after the pressure in the methyl phosphine aldehyde reaction liquid continuous evaporation and concentration device is normal pressure, the nitrogen inlet pipeline is closed, the vacuum pump 10 is started to pump negative pressure, after evacuation is finished, the nitrogen inlet pipeline 109 is opened for gas replacement, the operation is repeated for many times, and finally the whole device is in a nitrogen protection state.
The 1# methyl phosphine aldehyde storage tank 4 and the 2# methyl phosphine aldehyde storage tank 5 are mutually standby, are provided with liquid level meters and have a high liquid level alarm function. The No. 1 liquid phase outlet pipeline 103 is provided with an electromagnetic valve and is interlocked with a liquid level meter signal on the No. 1 methyl phosphine aldehyde storage tank 4; the 2# liquid phase outlet pipeline 104 is also provided with an electromagnetic valve which is interlocked with a liquid level meter signal on the 2# methylphosphine aldehyde storage tank 5. When any storage high liquid level exists in the 1# methylphosphine aldehyde storage tank 4 and the 2# methylphosphine aldehyde storage tank 5, the functions of closing the electromagnetic valve communicated with the storage tanks and opening the electromagnetic valve communicated with the other storage tank are achieved, and therefore continuous evaporation of the methylphosphine aldehyde reaction liquid is achieved.
No. 1 concentrate receiving tank 8 and No. 2 concentrate receiving tank 9 each other reserve, all be provided with the level gauge, possess high liquid level alarming function. The primary condensate outlet pipeline 107 is provided with an electromagnetic valve which is interlocked with a signal of a liquid level meter on the No. 1 concentrated solution receiving tank 8; the condensate inlet conduit 109 is also provided with a solenoid valve interlocked with the level gauge signal in the # 2 concentrate receiving tank 9. When any one of the concentrated solution receiving tank 1# 8 and the concentrated solution receiving tank 2# 9 has a high storage liquid level, the functions of closing the electromagnetic valve communicated with the storage tank and opening the electromagnetic valve communicated with the other storage tank are achieved, and therefore the methyl phosphine aldehyde reaction liquid is continuously evaporated.
Example 1:
the components of the methyl phosphine aldehyde reaction liquid are 45 percent of methyl phosphine aldehyde, 28.5 percent of ethanol and 26.5 percent of water according to weight percentage.
The structure of the apparatus for carrying out continuous evaporation and concentration of the methylphosphine aldehyde reaction solution is shown in FIG. 1. Under the operation of the water ring vacuum pump, the vacuum degree in the whole methyl phosphine aldehyde reaction liquid continuous evaporation concentration device is controlled at-10 kPa, and the heat exchange area of the heat exchange jacket at the side part of the film evaporator 3 is 15m2The heating medium is steam, and the evaporation temperature of the liquid in the thin film evaporator 3 is controlled to be between 80 and 82 ℃ by adjusting the opening degree of a No. 5 electromagnetic valve on a heating medium inlet pipeline.
The delivery pump 2 is a shield pump with a maximum delivery capacity of 3m3H, controlling the feeding amount of the methyl phosphine aldehyde reaction liquid to be 2m by adjusting the opening of a control valve on an outlet pipeline 102 of the conveying pump3/h。
The reaction liquid storage tank 1 is a vertical container made of steel lining PO with a volume of 10m3. The 1# methylphosphinic aldehyde storage tank 4 and the 2# methylphosphinic aldehyde storage tank 5 are both vertical storage tanks, are made of stainless steel and have the volume of 10m3. The No. 1 concentrated solution receiving tank 8 and the No. 2 concentrated solution receiving tank 9 are vertical storage tanks, are made of steel lining PO, and have a volume of 10m3。
The first-stage gas phase condenser 6 is a horizontal heat exchanger, the condensing medium is circulating water, the temperature of a gas phase outlet at the upper part of a heat channel of the first-stage gas phase condenser 6 is controlled to be 40 ℃, and the heat exchange area is 40m2. The two-stage gas phase condenser 7 is a horizontal heat exchanger, the condensing medium is frozen brine, and the heat exchange area is 30m2。
Tests show that the purity of the methyl phosphine aldehyde in the 1# methyl phosphine aldehyde storage tank 4 and the 2# methyl phosphine aldehyde storage tank 5 is 98.2 percent, and the removal efficiency of the ethanol in the methyl phosphine aldehyde reaction liquid is 97 percent.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (7)
1. The continuous methyl phosphine aldehyde reaction liquid evaporation and concentration device is characterized in that: the device comprises a thin film evaporator (3), wherein a liquid inlet at the upper part of the thin film evaporator (3) is sequentially connected with a conveying pump (2) and a reaction liquid storage tank (1) through pipelines, a stirrer for stirring liquid in the thin film evaporator (3) is arranged at the top of the thin film evaporator, a gas outlet at the upper part of the thin film evaporator (3) is sequentially connected with a gas condensation and collection device and a vacuum pump (10) through pipelines, the vacuum state in the thin film evaporator (3) is maintained under the operation action of the vacuum pump (10), and the gas condensation and collection device is used for condensing and collecting a gas phase solvent flowing out of the gas outlet at the upper part of the thin film evaporator; a liquid outlet at the bottom of the thin film evaporator (3) is divided into two paths, one path is connected with a 1# methylphosphine aldehyde storage tank (4) through a 1# liquid phase outlet pipeline (103), and the other path is connected with a 2# methylphosphine aldehyde storage tank (5) through a 2# liquid phase outlet pipeline (104); the 1# electromagnetic valve and the 2# electromagnetic valve are respectively arranged on the 1# liquid phase outlet pipeline (103) and the 2# liquid phase outlet pipeline (104), the 1# liquid level meter and the 2# liquid level meter are respectively arranged on the 1# methyl phosphine aldehyde storage tank (4) and the 2# methyl phosphine aldehyde storage tank (5), and the 1# liquid level meter and the 2# liquid level meter are both in signal connection with the 1# electromagnetic valve and the 2# electromagnetic valve through a PLC control system;
when the 1# liquid level meter measures that the liquid level in the 1# methylphosphine aldehyde storage tank (4) reaches a set liquid level, transmitting a liquid level signal to a PLC control system, and feeding back and controlling the 1# electromagnetic valve to be closed and the 2# electromagnetic valve to be opened through the PLC control system; when the 2# liquid level meter measures that the liquid level in the 2# methyl phosphine aldehyde storage tank (5) reaches a set liquid level, a liquid level signal is transmitted to the PLC control system, the 2# electromagnetic valve is controlled to be closed and the 1# electromagnetic valve is controlled to be opened through feedback of the PLC control system, therefore, the 1# methyl phosphine aldehyde storage tank (4) and the 2# methyl phosphine aldehyde storage tank (5) are mutually standby, when one is in a liquid storage state, the other is discharged, and therefore continuous evaporation of the methyl phosphine aldehyde reaction liquid is achieved; control valves are arranged on the corresponding pipelines.
2. The continuous evaporation and concentration device of methyl phosphine aldehyde reaction liquid as claimed in claim 1, wherein: the gas condensation and collection device comprises a first-stage gas phase condenser (6), a No. 1 concentrated solution receiving tank (8) and a second-stage gas phase condenser (7), wherein the first-stage gas phase condenser (6) and the second-stage gas phase condenser (7) are both in heat exchanger structures, a gas outlet in the upper part of the film evaporator (3) is connected with an inlet of the first-stage gas phase condenser (6) through a gas outlet pipeline (105), a gas outlet in the upper part of the first-stage gas phase condenser (6) is connected with the second-stage gas phase condenser (7) through a non-condensable gas outlet pipeline (106), and a gas outlet in the upper part of the second-stage gas phase condenser (7) is connected with a;
the liquid phase outlet at the bottom of the primary gas phase condenser (6) is connected with the 1# concentrated solution receiving tank (8) through a primary condensate outlet pipeline (107), and the liquid phase outlet at the bottom of the secondary gas phase condenser (7) is connected with the primary condensate outlet pipeline (107) through a secondary condensate outlet pipeline (108) so as to collect the solvent concentrated solution condensed by the primary gas phase condenser (6) and the secondary gas phase condenser (7) into the 1# concentrated solution receiving tank (8) respectively.
3. The continuous evaporation and concentration device of methyl phosphine aldehyde reaction liquid as claimed in claim 2, wherein: the device also comprises a No. 2 concentrated solution receiving tank (9), wherein a liquid inlet at the top of the No. 2 concentrated solution receiving tank (9) is connected with a primary condensate outlet pipeline (107) through a condensate inlet pipeline (109); a 3# electromagnetic valve is arranged on a primary condensate outlet pipeline (107) between the condensate inlet pipeline (109) and the 1# concentrated solution receiving tank (8), a 4# electromagnetic valve is arranged on the condensate inlet pipeline (109), a 3# liquid level meter and a 4# liquid level meter are respectively arranged on the 1# concentrated solution receiving tank (8) and the 2# concentrated solution receiving tank (9), and the 3# liquid level meter and the 4# liquid level meter are in signal connection with the 3# electromagnetic valve and the 4# electromagnetic valve through a PLC control system;
when the 3# liquid level meter measures that the liquid level in the 1# concentrated liquid receiving groove (8) reaches a set liquid level, a liquid level signal is transmitted to the PLC control system, and the 3# electromagnetic valve is fed back and controlled to be closed and the 4# electromagnetic valve is controlled to be opened through the PLC control system; when the 4# liquid level meter measures that the liquid level in the 2# concentrated solution receiving groove (9) reaches a set liquid level, a liquid level signal is transmitted to the PLC control system, the 4# electromagnetic valve is controlled to be closed and the 3# electromagnetic valve is controlled to be opened through feedback of the PLC control system, therefore, the 1# concentrated solution receiving groove (8) and the 2# concentrated solution receiving groove (9) are mutually standby, when one is in a liquid storage state, the other is used for discharging liquid, and therefore continuous evaporation of the methyl phosphine aldehyde reaction liquid is achieved;
the liquid outlets at the bottoms of the 1# concentrated solution receiving tank (8) and the 2# concentrated solution receiving tank (9) are connected with a condensate recovery pipeline (119) through a branch pipe provided with a control valve, and the concentrated solvent solution collected in the 1# concentrated solution receiving tank (8) or the 2# concentrated solution receiving tank (9) is sent to a solvent recovery system through the condensate recovery pipeline (119) for refining and recycling.
4. The continuous evaporation and concentration device of methyl phosphine aldehyde reaction liquid as claimed in claim 2, wherein: the primary gas-phase condenser (6) and the secondary gas-phase condenser (7) are both of heat exchanger structures, the inlet and the outlet of a cold channel of the primary gas-phase condenser (6) are respectively communicated with a primary condensing medium inlet pipeline (115) and a primary condensing medium outlet pipeline (116), the inlet and the outlet of the cold channel of the secondary gas-phase condenser (7) are respectively communicated with a secondary condensing medium inlet pipeline (117) and a secondary condensing medium outlet pipeline (118), and condensing media are respectively introduced into the cold channel of the primary gas-phase condenser (6) and the cold channel of the secondary gas-phase condenser (7); vacuum pump inlet pipeline (110) expert is connected with nitrogen gas inlet pipeline (111), and 1# concentrate receiving tank (8) top is passed through gaseous phase equilibrium pipeline (112) and is connected with vacuum pump inlet pipeline (110), and 2# concentrate receiving tank (9) top is passed through a branch pipe and is connected with gaseous phase equilibrium pipeline (112).
5. The continuous evaporation and concentration device of methyl phosphine aldehyde reaction liquid as claimed in claim 1, wherein: the reaction liquid storage tank (1) is vertical, is made of PO (stainless steel) lined with steel, carbon steel or stainless steel, and has a volume of 5-30 m3To (c) to (d); the delivery pump (2) is a canned motor pump, a pneumatic diaphragm pump or a metering pump, the outlet of the delivery pump (2) is connected with the liquid inlet at the upper part of the film evaporator (3) through an outlet pipeline (102), the outlet pipeline (102) of the delivery pump is provided with a flow meter, a control valve and a control valveThe flow rate of the methyl phosphine aldehyde reaction liquid conveyed into the film evaporator (3) is 1-5 m3/h；
The No. 1 methyl phosphine aldehyde storage tank (4) or the No. 2 methyl phosphine aldehyde storage tank (5) is made of PO lined with steel, carbon steel, stainless steel or glass lining, and has a volume of 5-30 m3In the meantime.
6. The continuous evaporation and concentration device of methyl phosphine aldehyde reaction liquid as claimed in claim 1, wherein: the thin film evaporator (3) is provided with a thermometer for measuring the temperature of liquid inside the thin film evaporator, the side part of the thin film evaporator (3) is sleeved with a heat exchange jacket, an inlet and an outlet of the heat exchange jacket are respectively communicated with a heating medium inlet pipeline (113) and a heating medium outlet pipeline (114), a heating medium introduced into the heat exchange jacket is high-temperature steam or hot water, and the heat exchange area of the heat exchange jacket is 2-20 m2(ii) a The heating medium inlet pipeline (113) is provided with a No. 5 electromagnetic valve, the No. 5 electromagnetic valve is in signal connection with a thermometer on the thin film evaporator (3) through a PLC control system, the thermometer transmits the measured liquid temperature to the PLC control system, and the opening of the No. 5 electromagnetic valve is fed back and controlled through the PLC control system so as to adjust and control the liquid phase temperature in the thin film evaporator (3).
7. The continuous evaporation and concentration device of methylphosphine aldehyde reaction solution according to claim 4, wherein: the condensing medium introduced into the cold channel of the first-stage gas phase condenser (6) is circulating water, low-temperature water or frozen brine, and the heat exchange area of the condensing medium is 10-50 m2(ii) a The condensing medium introduced into the cold channel of the secondary gas phase condenser (7) is low-temperature water or frozen brine, and the heat exchange area of the condensing medium is 5-40 m2(ii) a The No. 1 concentrated solution receiving tank (8) or the No. 2 concentrated solution receiving tank (9) is made of PO lined with steel, carbon steel or stainless steel, and the volume of the tank is 5-30 m3In the meantime.
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| CN202020874228.4U CN212347747U (en) | 2020-05-22 | 2020-05-22 | Methyl phosphine aldehyde reaction liquid continuous evaporation and concentration device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111569450A (en) * | 2020-05-22 | 2020-08-25 | 浙江省天正设计工程有限公司 | Methyl phosphine aldehyde reaction liquid continuous evaporation concentration device and concentration process |
| WO2024103424A1 (en) * | 2022-11-15 | 2024-05-23 | 岳阳景嘉化工有限公司 | Cryogenic exhaust gas removal material apparatus |
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2020
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111569450A (en) * | 2020-05-22 | 2020-08-25 | 浙江省天正设计工程有限公司 | Methyl phosphine aldehyde reaction liquid continuous evaporation concentration device and concentration process |
| CN111569450B (en) * | 2020-05-22 | 2023-12-26 | 浙江省天正设计工程有限公司 | Continuous evaporation concentration device and concentration process for methylphosphonic aldehyde reaction liquid |
| WO2024103424A1 (en) * | 2022-11-15 | 2024-05-23 | 岳阳景嘉化工有限公司 | Cryogenic exhaust gas removal material apparatus |
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Effective date of registration: 20211230 Address after: 311600 Xin'anjiang Town, Jiande City, Hangzhou City, Zhejiang Province Patentee after: ZHEJIANG WYNCA CHEMICAL INDUSTRY GROUP Co.,Ltd. Address before: 310012 Building 2, golden Xixi, 199 Shuanglong street, Xihu District, Hangzhou City, Zhejiang Province Patentee before: ZHEJIANG TITAN DESIGN & ENGINEERING Co.,Ltd. |