CN114832753B - Device and method for continuously preparing orthoformate - Google Patents
Device and method for continuously preparing orthoformate Download PDFInfo
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- CN114832753B CN114832753B CN202210645337.2A CN202210645337A CN114832753B CN 114832753 B CN114832753 B CN 114832753B CN 202210645337 A CN202210645337 A CN 202210645337A CN 114832753 B CN114832753 B CN 114832753B
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
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- B01J4/00—Feed or outlet devices; Feed or outlet control devices
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Abstract
The application provides a device and a method for continuously preparing orthoformate, comprising a continuous salifying reaction kettle, a continuous salifying heat preservation kettle, a vacuum dechlorination tower, a continuous alcoholysis kettle, a centrifugal elevated tank, a centrifugal separator and a crude product storage tank which are sequentially connected, wherein the top of the vacuum dechlorination tower is sequentially connected with a vacuum buffer tank and a vacuum unit, the continuous salifying reaction kettle is communicated with a first circulating condenser, the continuous salifying heat preservation kettle is communicated with a second circulating condenser, and the continuous alcoholysis kettle is communicated with a circulating heater. According to the device for continuously preparing the orthoformate, provided by the application, the raw material liquid is continuously added into the continuous salifying reaction kettle to generate salifying material liquid, dechlorination treatment is carried out through the vacuum dechlorination tower, the salifying material liquid is sent into the continuous alcoholysis kettle to carry out alcoholysis reaction, and finally, the crude orthoformate is obtained through centrifugal separation, so that continuous production of the orthoformate can be realized, the amount of hydrocyanic acid added in unit time is reduced in multiple, and the safety is ensured.
Description
Technical Field
The application belongs to the technical field of orthoformate reaction equipment, and particularly relates to a device and a method for continuously preparing orthoformate.
Background
The orthoformate is an important intermediate raw material liquid for organic chemical industry, is widely applied to the fields of pesticides, medicines, synthetic materials and the like, is an important raw material liquid for synthesizing substances such as azoxystrobin, medicinal antimalarial drugs chloroquine, quinine and the like, and has high use value.
At present, an intermittent reaction kettle is mainly adopted for producing orthoformate, the equipment quantity is large, the production efficiency is low, and the labor intensity is high. Particularly, in the salification reaction, the main raw material liquid is hydrocyanic acid, the hydrocyanic acid belongs to highly toxic substances, the problems of large material feeding amount and severe reaction heat release exist in the intermittent reaction process, the high-temperature material flushing accident is difficult to control, and the safety problem is outstanding.
Disclosure of Invention
The application aims to provide a device and a method for continuously preparing orthoformate, which can reduce the one-time feeding amount of hydrocyanic acid through a continuous reaction device and improve the safety in the process of preparing the orthoformate.
In order to achieve the above purpose, the application adopts the following technical scheme: the device comprises a continuous salifying reaction kettle, a continuous salifying heat preservation kettle, a vacuum dechlorination tower, a continuous alcoholysis kettle, a centrifugal elevated tank, a centrifugal separator and a crude product storage tank which are sequentially connected, wherein the continuous salifying reaction kettle is used for continuously receiving raw material liquid and producing salified material liquid, the vacuum dechlorination tower is used for receiving salified material liquid and dechlorinating to form dechlorinated material liquid, the continuous alcoholysis kettle is used for receiving dechlorinated material liquid and alcoholysis to form alcoholysis material liquid, the top of the vacuum dechlorination tower is sequentially connected with a vacuum buffer tank and a vacuum unit, a first circulating condenser for cooling is communicated with the continuous salifying reaction kettle, a second circulating condenser for cooling is communicated with the continuous salifying heat preservation kettle, and a circulating heater for heating is communicated with the continuous alcoholysis kettle.
In one possible implementation manner, the continuous salifying reaction kettle, the continuous salifying heat preservation kettle, the continuous alcoholysis kettle and the centrifugal elevated tank are respectively provided with a stirring assembly, and the stirring assembly comprises:
the stirring shaft is rotationally connected in the continuous salifying heat preservation kettle, the centrifugal elevated tank or the continuous alcoholysis kettle along the up-down direction;
the paddle stirring blades are respectively connected to the periphery of the upper part of the stirring shaft and are uniformly distributed on the periphery of the stirring shaft;
the anchor stirring blades are connected to the periphery of the lower end of the stirring shaft and uniformly distributed on the periphery of the stirring shaft, and the outer ends of the anchor stirring blades gradually incline upwards outwards.
In one possible implementation, the continuous salifying reaction kettles are respectively provided with a distributor, and the distributor is provided with a solvent back flushing pipe.
In some embodiments, the continuous salifying reaction kettles are respectively provided with a distributor, and a solvent backwash pipe is arranged on the distributor.
In some embodiments, the stirring shaft in the continuous salifying reaction kettle is a hollow shaft, self-priming paddles are further arranged on the periphery of the hollow shaft, and a plurality of air extraction holes for extracting unreacted hydrogen chloride gas are formed on the periphery of the upper part of the hollow shaft;
the self-priming blade is communicated with the interior of the hollow shaft, and the outer wall of the self-priming blade is provided with an air outlet hole for forming a negative pressure environment and enabling hydrogen chloride gas in the hollow shaft to enter the raw material liquid.
In one possible implementation manner, the top of the vacuum dechlorination tower is provided with a pressure transmitter and a controller electrically connected with the pressure transmitter, the vacuum unit is provided with a frequency converter electrically connected with the controller, the frequency converter is used for assisting the vacuum unit to adjust the vacuum degree in the vacuum dechlorination tower, and the vacuum unit is a liquid ring vacuum pump or a screw vacuum pump.
In some embodiments, the vacuum unit further comprises at least one Roots vacuum pump connected between the vacuum unit and the vacuum buffer tank.
In one possible implementation mode, a material distribution assembly connected with a discharging pipe of the continuous salifying heat insulation kettle is arranged in the vacuum dechlorination tower, the material distribution assembly comprises a plurality of atomizing spray heads positioned at the upper part of the vacuum dechlorination tower, and a cyclone foam remover positioned above the atomizing spray heads is also arranged in the vacuum dechlorination tower.
In one possible implementation manner, a first circulating pump connected with a first circulating condenser and a salt-forming extraction pump for feeding salt-forming feed liquid into the continuous salt-forming heat-preserving kettle are arranged on a discharge pipe of the continuous salt-forming reaction kettle;
a second circulating pump connected with the second circulating condenser and a heat-preserving extraction pump for feeding salt forming feed liquid into the vacuum dechlorination tower are arranged on a discharge pipe of the continuous salt forming heat-preserving kettle;
and a third circulating pump connected with the circulating heater and an alcoholysis extraction pump used for feeding alcoholysis feed liquid into the centrifugal overhead tank are arranged on the discharge pipe of the continuous alcoholysis kettle.
Compared with the prior art, the device for continuously preparing the orthoformate provided by the embodiment of the application has the advantages that raw material liquid is continuously added into the continuous salifying reaction kettle, the generated salifying material liquid is sent into the continuous salifying heat preservation kettle for a certain period of time, then dechlorination treatment is carried out through the vacuum dechlorination tower, the dechlorinated material liquid is sent into the continuous alcoholysis kettle for alcoholysis reaction, and finally centrifugal separation is carried out to obtain the crude orthoformate, so that continuous production of the orthoformate is realized, the equipment quantity is convenient to reduce, the hydrocyanic acid amount added in unit time is reduced in a multiplied mode, and the safety problem is effectively ensured.
The application also provides a method for preparing orthoformate by using the device for continuously preparing orthoformate, which comprises the following steps:
respectively adding a solvent into a continuous salification reaction kettle, a continuous salification heat preservation kettle and a continuous alcoholysis kettle;
continuously feeding four raw material liquids of hydrocyanic acid, alcohol, hydrogen chloride and solvent into a continuous salifying reaction kettle according to a preset proportion, stirring and reacting to generate salifying material liquid, and controlling the temperature of the continuous salifying reaction kettle to be in a range of 25-30 ℃;
when the liquid level of the continuous salifying reaction kettle is higher than a first preset liquid level, feeding salifying liquid to the continuous salifying heat preservation kettle, and preserving heat in the continuous salifying heat preservation kettle for 4 hours;
when the liquid level of the continuous salifying heat preservation kettle is higher than a second preset liquid level, feeding salifying liquid into a vacuum dechlorination tower, controlling the vacuum degree of the vacuum dechlorination tower to be more than minus 0.09Mpa, and removing excessive hydrogen chloride and alcohol to obtain dechlorinated liquid;
when the liquid level of the vacuum dechlorination tower is higher than a third preset liquid level, feeding dechlorination feed liquid to a continuous alcoholysis kettle, adding alcohol in equal proportion, and controlling the temperature of the continuous alcoholysis kettle to be within the range of 55-60 ℃;
when the liquid level of the continuous alcoholysis kettle is higher than a fourth preset liquid level, feeding alcoholysis liquid to a centrifugal separator through a centrifugal elevated tank, continuously separating alcoholysis liquid by the centrifugal separator to obtain solid ammonium chloride and crude orthoformate, and feeding crude orthoformate to a crude orthoformate storage tank.
In some embodiments, in the step of adding solvent to the continuous salification reaction kettle, the continuous salification heat preservation kettle and the continuous alcoholysis kettle respectively, adding solvent to the continuous salification reaction kettle from half of the maximum volume in the continuous salification reaction kettle to the continuous salification reaction kettle; adding solvent into the continuous salification heat-insulation kettle from half of the maximum volume of the continuous salification heat-insulation kettle; adding a solvent into the continuous alcoholysis kettle from half of the maximum volume of the continuous alcoholysis kettle;
in the step of continuously feeding four raw material liquids of hydrocyanic acid, alcohol, hydrogen chloride and solvent into a continuous salifying reaction kettle, the weight ratio of the hydrocyanic acid to the alcohol to the hydrogen chloride to the solvent is 1 (1.1-1.3) (1.4-1.6) (8.5-9.5).
Compared with the prior art, the scheme provided by the embodiment of the application has the advantages that the raw material liquid is continuously input, and the crude product of the orthoformate is continuously prepared by sequentially carrying out salt forming reaction, dechlorination reaction, alcoholysis reaction and centrifugal separation, so that the continuous production of the orthoformate is realized, the equipment quantity is convenient to reduce, the input hydrocyanic acid amount in unit time is reduced by times, and the safety problem is effectively ensured.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of an apparatus for continuously preparing orthoformate according to an embodiment of the present application;
fig. 2 is a schematic structural diagram of the continuous salt-forming thermal insulation kettle in fig. 1 according to an embodiment of the present application.
Wherein, each reference sign in the figure:
1. a continuous salification reaction kettle; 11. a first recycle condenser; 12. self-priming paddle; 13. a salification extraction pump; 14. a first circulation pump; 2. a continuous salification heat preservation kettle; 21. a second recycle condenser; 22. a second circulation pump; 23. a thermal insulation extraction pump; 3. a vacuum dechlorination tower; 31. a vacuum buffer tank; 32. a vacuum unit; 33. an atomizing nozzle; 34. a cyclone demister; 4. a continuous alcoholysis kettle; 41. a circulation heater; 42. a third circulation pump; 43. an alcoholysis extraction pump; 5. centrifuging the elevated tank; 6. a centrifugal separator; 7. a crude product storage tank; 81. a stirring assembly; 82. a distributor; 83. a stirring shaft; 84. paddle stirring blades; 85. anchor stirring vane.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
It will be understood that when an element is referred to as being "disposed on" another element, it can be directly on the other element or be indirectly on the other element. It is to be understood that the terms "length," "width," "upper," "lower," "front," "rear," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate describing the present application and simplify the description, and do not indicate or imply that the devices or elements being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be construed as limiting the present application. The terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a number" is two or more, unless explicitly defined otherwise.
Referring to fig. 1 to 2, an apparatus and a method for continuously preparing orthoformate according to the present application will now be described. The device for continuously preparing the orthoformate comprises a continuous salifying reaction kettle 1, a continuous salifying heat preservation kettle 2, a vacuum dechlorination tower 3, a continuous alcoholysis kettle 4, a centrifugal elevated tank 5, a centrifugal separator 6 and a crude product storage tank 7 which are sequentially connected, wherein the continuous salifying reaction kettle 1 is used for continuously receiving raw material liquid and producing salified material liquid, the vacuum dechlorination tower 3 is used for receiving salified material liquid and dechlorinating to form dechlorinated material liquid, the continuous alcoholysis kettle 4 is used for receiving dechlorinated material liquid and alcoholysis to form alcoholysis material liquid, the top of the vacuum dechlorination tower 3 is sequentially connected with a vacuum buffer tank 31 and a vacuum unit 32, a first circulating condenser 11 for cooling is communicated with the continuous salifying reaction kettle 1, a second circulating condenser 21 for cooling is communicated with the continuous salifying heat preservation kettle 2, and a circulating heater 41 for heating is communicated with the continuous alcoholysis kettle 4.
Compared with the prior art, the device for continuously preparing the orthoformate provided by the embodiment is characterized in that raw material liquid is continuously added into the continuous salifying reaction kettle 1, the generated salifying material liquid is sent into the continuous salifying heat preservation kettle 2 for a certain period of time for heat preservation, the dechlorination treatment is carried out through the vacuum dechlorination tower 3, the dechlorination material liquid is then sent into the continuous alcoholysis kettle 4 for alcoholysis reaction, and finally centrifugal separation is carried out to obtain crude orthoformate, so that continuous production of the orthoformate is realized, the equipment quantity is reduced conveniently, the hydrocyanic acid amount added in unit time is reduced in a multiplied mode, and the safety problem is effectively guaranteed.
In the embodiment, the continuous salification heat preservation kettle 2 has a similar structure to the continuous salification reaction kettle 1, and is used for carrying out heat preservation treatment on salification liquid produced by reaction, ensuring that hydrocyanic acid can be completely reacted, and reducing the safety risk in the production process.
Specifically, in the above-described apparatus, the continuous salifying reaction vessel 1, the continuous salifying thermal insulation vessel 2, the continuous alcoholysis vessel 4, and the centrifugal overhead tank 5 are stainless steel members, respectively. The stainless steel material has good corrosion resistance, and is convenient for prolonging the service life of equipment. The centrifugal separator 6 is a continuously operated pusher centrifuge, a spiral decanter centrifuge or a flat-plate lower discharge centrifuge.
In some possible implementations, the continuous alcoholysis tank 4 and the centrifugal elevated tank 5 are constructed as shown in fig. 1. Referring to fig. 1, a continuous salifying reaction kettle 1, a continuous salifying heat preservation kettle 2, a continuous alcoholysis kettle 4 and a centrifugal overhead tank 5 are respectively provided with a stirring assembly 81, wherein the stirring assembly 81 comprises a stirring shaft 83, a plurality of paddle stirring blades 84 and a plurality of anchor stirring blades 85, and the stirring shaft 83 is rotationally connected in the vertical direction in the continuous salifying heat preservation kettle 2, the centrifugal overhead tank 5 or the continuous alcoholysis kettle 4; the paddle stirring blades 84 are respectively connected to the upper periphery of the stirring shaft 83, and are uniformly distributed on the periphery of the stirring shaft 83; the anchor stirring blades 85 are connected to the periphery of the lower end of the stirring shaft 83, and are uniformly distributed on the periphery of the stirring shaft 83, and the outer ends of the anchor stirring blades 85 gradually incline upwards and outwards.
In this embodiment, stirring assemblies 81 are respectively disposed in the continuous salifying reaction kettle 1, the continuous salifying heat preservation kettle 2, the continuous alcoholysis kettle 4 and the centrifugal overhead tank 5, and the stirring assemblies 81 in the four devices have the same structure and are in a form of combining a paddle stirring blade 84 and an anchor stirring blade 85.
The stirring unit 81 in the continuous alcoholysis tank 4 is exemplified. The paddle stirring vane 84 in the continuous alcoholysis kettle 4 is mainly used for stirring the raw material liquid in the middle area of the continuous alcoholysis kettle 4, and the anchor stirring vane 85 is arranged at the lower end of the stirring shaft 83 and used for stirring the raw material liquid in the position, close to the bottom, of the continuous alcoholysis kettle 4, so that the anchor stirring vane 85 and the bottom wall of the continuous alcoholysis kettle 4 are prevented from being interfered in position, solid materials can be effectively distributed in the raw material liquid, and meanwhile, the solid materials are prevented from settling and blocking a blanking pipeline, the stirring efficiency is improved, and the stirring uniformity is ensured. Specifically, the two layers of paddle stirring blades 84 are arranged in the continuous alcoholysis kettle 4, so that raw material liquids at different height positions in the kettle can be sufficiently stirred, and the stirring efficiency is improved.
In some possible implementations, the continuous salification reaction kettle 1 and the continuous salification heat-preservation kettle 2 with the characteristics adopt structures as shown in fig. 2. Referring to fig. 2, a distributor 82 is further arranged in the continuous salifying reaction kettle 1, and a solvent back flushing pipe is arranged on the distributor 82.
In order to enable the raw material liquid to fully react in the continuous salifying reaction kettle 1, when the raw material liquid is added into the continuous salifying reaction kettle 1, the distributor 82 is utilized to uniformly distribute hydrocyanic acid, hydrogen chloride and alcohol, so that effective contact of the hydrocyanic acid, the hydrogen chloride and the alcohol can be realized, and an imine salt can be quickly generated, namely, the salifying material liquid, the uniformity of the cloth is improved, and the salifying material liquid with complete reaction can be conveniently obtained.
In order to avoid blockage of the distributor 82 caused by accumulation of the raw material liquid on the distributor 82, a solvent backwash tube is further arranged on the distributor 82, so that timing backwash can be realized, and blockage of the distributor 82 by the salified material liquid is prevented.
In some embodiments, referring to fig. 2, the stirring shaft 83 in the continuous salifying reaction kettle 1 is a hollow shaft, the periphery of the hollow shaft is also provided with self-priming paddles 12, and the periphery of the upper part of the hollow shaft is provided with a plurality of air extraction holes 131 for extracting unreacted hydrogen chloride gas;
the self-priming blade 12 is communicated with the inside of the hollow shaft, and the outer wall of the self-priming blade 12 is provided with an air outlet 141 for forming a negative pressure environment and enabling the hydrogen chloride gas in the hollow shaft to enter the raw material liquid.
The stirring shaft 83 adopts a hollow shaft structure, the self-priming blade 12 has a self-priming function in the stirring process, and unreacted hydrogen chloride gas above the raw material liquid can be sucked into the hollow shaft through the air suction holes 131 during stirring operation and is distributed into the material liquid through the air outlet holes 141 on the self-priming blade 12 so as to carry out subsequent full reaction.
On the basis of the structure, a baffle plate is further arranged in the continuous salifying reaction kettle 1 and used for further baffling and disturbing the raw material liquid, so that the raw material liquid is effectively and uniformly distributed, and the reaction efficiency of the materials is improved.
In some possible implementations, the above-mentioned characteristic vacuum dechlorination tower 3 adopts a structure as shown in fig. 1. Referring to fig. 1, a pressure transmitter and a controller electrically connected with the pressure transmitter are arranged at the top of the vacuum dechlorination tower 3, a frequency converter electrically connected with the controller is arranged on the vacuum unit 32, the frequency converter is used for assisting the vacuum unit 32 to adjust the vacuum degree in the vacuum dechlorination tower 3, and the vacuum unit 32 is a liquid ring vacuum pump or a screw vacuum pump.
A pressure transducer is a device that converts pressure into a pneumatic or electric signal for control and remote transmission. In this embodiment, the pressure transmitter converts the physical pressure parameter sensed by the load cell sensor into a standard electrical signal, and transmits the detected pressure parameter to the controller, the controller compares the pressure parameter with the preset pressure parameter according to a preset program, judges that the vacuum degree in the vacuum dechlorination tower 3 needs to be raised or lowered, and then the controller sends a control signal to the frequency converter to raise or lower the output frequency of the frequency converter, so as to further realize the regulation of the vacuum degree in the vacuum dechlorination tower 3 by the vacuum unit 32, so that the vacuum degree in the vacuum dechlorination tower 3 is kept within a certain range, and the vacuum dechlorination effect is satisfied.
In some embodiments, the feature vacuum unit 32 may be configured as shown in fig. 2. Referring to fig. 2, the vacuum unit 32 further includes at least one roots vacuum pump connected between the vacuum unit 32 and the vacuum buffer tank 31.
In this embodiment, the vacuum degree of the vacuum unit 32 is increased by the roots vacuum pump. The Roots vacuum pump has two vane-shaped rotors rotating synchronously in opposite directions, and has small gaps between the rotors and the inner wall of the pump casing.
In some possible implementations, the above-mentioned characteristic vacuum dechlorination tower 3 adopts a structure as shown in fig. 1. Referring to fig. 1, a material distribution assembly connected with a discharge pipe of the continuous salifying insulation kettle 2 is arranged in the vacuum dechlorination tower 3, the material distribution assembly comprises a plurality of atomizing spray heads 33 positioned at the upper part of the vacuum dechlorination tower 3, and a cyclone foam remover 34 positioned above the atomizing spray heads 33 is also arranged in the vacuum dechlorination tower 3.
In this embodiment, the vacuum dechlorination tower 3 carries out the even cloth of salt-forming liquid through the cloth subassembly of setting up inside top, and the cloth subassembly includes a plurality of atomizer 33, and atomizer 33 can be one or more, can fully disperse salt-forming liquid, is convenient for effectively deviate from unreacted complete hydrogen chloride and alcohol.
On the basis of the structure, the cyclone foam remover 34 positioned above the atomizing nozzle 33 is also arranged in the vacuum dechlorination tower 3, and the cyclone foam remover 34 prevents the foam from being entrained into the vacuum unit 32, so that the vacuum unit 32 is prevented from being damaged.
In some possible implementations, a first circulating pump 14 connected with the first circulating condenser 11 and a salt-forming extraction pump 13 for feeding salt-forming liquid into the continuous salt-forming heat-preserving kettle 2 are arranged on a discharge pipe of the continuous salt-forming reaction kettle 1;
a second circulating pump 22 connected with a second circulating condenser 21 and a heat-preserving extraction pump 23 for feeding salt forming liquid into the vacuum dechlorination tower 3 are arranged on a discharging pipe of the continuous salt forming heat-preserving kettle 2;
a third circulation pump 42 connected with the circulation heater 41 and an alcoholysis extraction pump 43 for feeding alcoholysis feed liquid into the centrifugal overhead tank 5 are arranged on the discharge pipe of the continuous alcoholysis tank 4.
In this embodiment, the first circulating condenser 11 and the second circulating condenser 21 are used to cool down the continuous salifying reaction kettle 1 and the continuous salifying heat preservation kettle 2 respectively, so that the stable reaction temperature is kept inside the continuous salifying reaction kettle and the continuous salifying heat preservation kettle, the reaction efficiency is improved, and the reaction quality is ensured.
Taking the continuous salifying reaction kettle 1 as an example, a first circulating pump 14 and a salifying extraction pump 13 are respectively connected to a discharge pipe of the continuous salifying reaction kettle 1, the first circulating pump 14 is used for bringing raw material liquid into the first circulating condenser 11, the raw material liquid is cooled in the first circulating condenser 11 and then is sent back to the continuous salifying reaction kettle 1 again, the cooling effect on the continuous salifying reaction kettle 1 is realized, the temperature in the continuous salifying reaction kettle 1 is kept within the range of 25-30 ℃, and the salified material liquid after the reaction is sent into the continuous salifying heat preservation kettle 2 under the action of the salifying extraction pump 13.
Similarly, the temperature in the continuous salt-forming reaction vessel 1 is also adjusted by the second circulation pump 22 and the heat-retaining extraction pump 23, and the temperature in the continuous alcoholysis vessel 4 is adjusted by the third circulation pump 42 and the alcoholysis extraction pump 43.
The first circulation pump 14, the second circulation pump 22 and the third circulation pump 42 are all forced circulation pumps, and a specific selectable high-flow mixed flow pump or an axial flow pump can effectively improve the flow velocity of the cooling medium or the heating medium in the tubes of the first condenser, the second condenser and the circulation heater 41 and prevent the tube array of the first condenser, the second condenser and the circulation heater 41 from being blocked by the wall-bonding of the salified feed liquid.
Based on the same inventive concept, the embodiment of the application also provides a method for preparing orthoformate by using the device for continuously preparing orthoformate, which comprises the following steps:
respectively adding solvent into a continuous salification reaction kettle 1, a continuous salification heat preservation kettle 2 and a continuous alcoholysis kettle 4;
continuously feeding four raw material liquids of hydrocyanic acid, alcohol, hydrogen chloride and solvent into a continuous salifying reaction kettle 1 according to a preset proportion, stirring and reacting to generate salifying material liquid, and controlling the temperature of the continuous salifying reaction kettle 1 to be in a range of 25-30 ℃;
when the liquid level of the continuous salifying reaction kettle 1 is higher than a first preset liquid level, feeding salifying liquid to the continuous salifying heat preservation kettle 2, and preserving heat for 4 hours in the continuous salifying heat preservation kettle 2;
when the liquid level of the continuous salifying heat preservation kettle 2 is higher than a second preset liquid level, feeding salifying liquid into a vacuum dechlorination tower 3, controlling the vacuum degree of the vacuum dechlorination tower 3 to be more than minus 0.09Mpa, and removing excessive hydrogen chloride and alcohol to obtain dechlorinated liquid;
when the liquid level of the vacuum dechlorination tower 3 is higher than a third preset liquid level, feeding dechlorination feed liquid to the continuous alcoholysis kettle 4, adding alcohol in equal proportion, and controlling the temperature of the continuous alcoholysis kettle 4 to be within the range of 55-60 ℃;
when the liquid level of the continuous alcoholysis kettle 4 is higher than a fourth preset liquid level, the alcoholysis liquid is fed to a centrifugal separator 6 through a centrifugal overhead tank 5, the centrifugal separator 6 continuously separates the alcoholysis liquid to obtain solid ammonium chloride and crude orthoformate, and the crude orthoformate is fed to a crude orthoformate storage tank 7.
In the continuous preparation process, firstly, a solvent which is half of the total amount of the required solvents is respectively added into a continuous salification reaction kettle 1, a continuous salification heat preservation kettle 2 and a continuous alcoholysis kettle 4 to be used as a base solution of continuous reaction. Then hydrocyanic acid, alcohol, hydrogen chloride and solvent are sent into a continuous salifying reaction kettle 1 according to the proportion of 1:1.2:1.5:9, the feeding process is metered by a mass flowmeter, the chain control is carried out through a pneumatic control valve, then stirring is carried out, meanwhile, a first circulating pump 14 is started, salifying feed liquid generated by the reaction is sent into a first circulating condenser 11, and the temperature of the continuous salifying reaction kettle 1 is controlled to be 25-30 ℃ through the control of the pneumatic control valve of the first circulating condenser 11.
The first circulating pump 14 is associated with the liquid level of the continuous salifying reaction kettle 1, when the actual liquid level is higher than the preset liquid level, salifying liquid is sent into the continuous salifying heat preservation kettle 2 through the salifying extraction pump 13, and stays in the continuous salifying heat preservation kettle 2 for 4 hours.
The heat-preserving extraction pump 23 is associated with the liquid level of the continuous salifying heat-preserving kettle 2, when the actual liquid level is higher than the preset liquid level, the heat-preserving extraction pump 23 sends salifying liquid into the vacuum dechlorination tower 3, and the vacuum degree of the vacuum dechlorination tower 3 is controlled to be more than minus 0.09Mpa so as to remove excessive hydrogen chloride and alcohol.
The discharge end of the vacuum dechlorination tower 3 is also provided with a vacuum extraction pump, the vacuum extraction pump is associated with the liquid level height in the vacuum dechlorination tower 3, the stability of the liquid level height in the vacuum dechlorination tower 3 is maintained, the vacuum extraction pump sends dechlorination feed liquid into the continuous alcoholysis kettle 4, meanwhile, alcohol is added according to the equal mass proportion, and the alcohol is metered through a mass flowmeter.
The third circulating pump 42 sends the alcoholysis feed liquid into the circulating heater 41 for heating, and the temperature in the alcoholysis reaction kettle is kept stable at 55-60 ℃. The alcoholysis extraction pump 43 is associated with the liquid level of the continuous alcoholysis tank 4, and when the actual liquid level is higher than the preset liquid level, the alcoholysis extraction pump 43 delivers the alcoholysis feed liquid into the centrifugal overhead tank 5 to keep the liquid level in the continuous alcoholysis tank 4 stable.
The centrifugal overhead tank 5 opens a discharging pneumatic valve to enable the feed liquid to enter the centrifugal separator 6 for continuous separation treatment, solid ammonium chloride is separated, the remaining mother liquid is crude orthoformate, the crude orthoformate enters the crude orthoformate storage tank 7 and is sent to a subsequent rectification system through a rectification and material pumping pump, and the finished orthoformate is obtained.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.
Claims (8)
1. The method for preparing the orthoformate by utilizing the device for continuously preparing the orthoformate is characterized in that the device for continuously preparing the orthoformate comprises a continuous salifying reaction kettle, a continuous salifying heat preservation kettle, a vacuum dechlorination tower, a continuous alcoholysis kettle, a centrifugal elevated tank, a centrifugal separator and a crude product storage tank which are sequentially connected, wherein the continuous salifying reaction kettle is used for continuously receiving raw material liquid and producing salified liquid, the vacuum dechlorination tower is used for receiving the salified liquid and dechlorinating to form dechlorinated liquid, the continuous alcoholysis kettle is used for receiving the dechlorinated liquid and alcoholysis to form alcoholysis liquid, the top of the vacuum dechlorination tower is sequentially connected with a vacuum buffer tank and a vacuum unit, the continuous salifying reaction kettle is communicated with a first circulating condenser for cooling down, the continuous salifying heat preservation kettle is communicated with a second circulating condenser for cooling down, and the continuous alcoholysis kettle is communicated with a circulating heater for heating up; a first circulating pump connected with the first circulating condenser and a salt-forming extraction pump used for feeding the salt-forming feed liquid into the continuous salt-forming heat-preserving kettle are arranged on a discharge pipe of the continuous salt-forming reaction kettle;
a second circulating pump connected with a second circulating condenser and a heat-preserving extraction pump for feeding the salified feed liquid into the vacuum dechlorination tower are arranged on a discharge pipe of the continuous salified heat-preserving kettle;
a third circulating pump connected with a circulating heater and an alcoholysis extraction pump used for supplying the alcoholysis feed liquid into the centrifugal overhead tank are arranged on a discharge pipe of the continuous alcoholysis kettle;
the method for preparing orthoformate comprises the following steps:
respectively adding solvents into the continuous salification reaction kettle, the continuous salification heat-preserving kettle and the continuous alcoholysis kettle;
continuously feeding four raw material liquids of hydrocyanic acid, alcohol, hydrogen chloride and solvent into the continuous salifying reaction kettle according to a preset proportion, stirring and reacting to generate salifying material liquid, and controlling the temperature of the continuous salifying reaction kettle to be in a range of 25-30 ℃;
when the liquid level of the continuous salifying reaction kettle is higher than a first preset liquid level, feeding salifying liquid to the continuous salifying heat preservation kettle, and preserving heat in the continuous salifying heat preservation kettle for 4 hours;
when the liquid level of the continuous salifying heat preservation kettle is higher than a second preset liquid level, feeding salifying liquid into a vacuum dechlorination tower, controlling the vacuum degree of the vacuum dechlorination tower to be more than minus 0.09Mpa, and removing excessive hydrogen chloride and alcohol to obtain dechlorinated liquid;
when the liquid level of the vacuum dechlorination tower is higher than a third preset liquid level, feeding dechlorination feed liquid to a continuous alcoholysis kettle, adding alcohol in equal proportion, and controlling the temperature of the continuous alcoholysis kettle to be within the range of 55-60 ℃;
when the liquid level of the continuous alcoholysis kettle is higher than a fourth preset liquid level, feeding the alcoholysis liquid to a centrifugal separator through a centrifugal overhead tank, continuously separating the alcoholysis liquid by the centrifugal separator to obtain solid ammonium chloride and crude orthoformate, and feeding the crude orthoformate to a crude orthoformate storage tank.
2. The method for preparing orthoformate according to claim 1, wherein each of the continuous salifying reaction kettle, the continuous salifying heat preservation kettle, the continuous alcoholysis kettle and the centrifugal overhead tank is provided with a stirring assembly, the stirring assembly comprising:
the stirring shaft is rotationally connected in the continuous salifying heat preservation kettle, the centrifugal elevated tank or the continuous alcoholysis kettle along the up-down direction;
the paddle stirring blades are respectively connected to the periphery of the upper part of the stirring shaft and are uniformly distributed on the periphery of the stirring shaft;
the anchor stirring blades are connected to the periphery of the lower end of the stirring shaft and are uniformly distributed on the periphery of the stirring shaft, and the outer ends of the anchor stirring blades gradually incline upwards outwards.
3. The method for preparing orthoformate according to claim 2, wherein the continuous salifying reaction kettles are respectively provided with a distributor, and a solvent backwash pipe is arranged on the distributor.
4. The method for preparing orthoformate according to claim 3, wherein the stirring shafts in the continuous salifying reaction kettle and the continuous salifying heat preservation kettle are hollow shafts, self-suction paddles are further arranged on the periphery of the hollow shafts, and a plurality of air extraction holes for extracting unreacted hydrogen chloride gas are formed on the periphery of the upper part of the hollow shafts;
the self-priming blade is communicated with the inside of the hollow shaft, and an air outlet hole used for forming a negative pressure environment and enabling the hydrogen chloride gas in the hollow shaft to enter the raw material liquid is formed in the outer wall of the self-priming blade.
5. The method for preparing orthoformate according to claim 1, wherein a pressure transmitter and a controller electrically connected with the pressure transmitter are arranged at the top of the vacuum dechlorination tower, a frequency converter electrically connected with the controller is arranged on the vacuum unit, the frequency converter is used for assisting the vacuum unit to adjust the vacuum degree in the vacuum dechlorination tower, and the vacuum unit is a liquid ring vacuum pump or a screw vacuum pump.
6. The method of making orthoformate of claim 5, wherein the vacuum train further includes at least one roots vacuum pump connected between the vacuum train and the vacuum buffer tank.
7. The method for preparing orthoformate according to any one of claims 1 to 6, wherein a distributing component connected with a discharging pipe of the continuous salifying thermal insulation kettle is arranged in the vacuum dechlorination tower, the distributing component comprises a plurality of atomizing spray heads positioned at the upper part of the vacuum dechlorination tower, and a cyclone foam remover positioned above the atomizing spray heads is also arranged in the vacuum dechlorination tower.
8. The method for producing orthoformate according to claim 1, wherein in the step of adding a solvent to the continuous salification reaction vessel, the continuous salification incubation vessel, and the continuous alcoholysis vessel, respectively, half of the maximum amount of the solvent in the continuous salification reaction vessel is added to the continuous salification reaction vessel; adding half of the maximum dosage of the solvent in the continuous salification heat-preserving kettle to the continuous salification heat-preserving kettle; adding half of the maximum dosage of the solvent in the continuous alcoholysis kettle to the continuous alcoholysis kettle;
in the step of continuously feeding the four raw material liquids of the hydrocyanic acid, the alcohol, the hydrogen chloride and the solvent into the continuous salifying reaction kettle, the weight ratio of the hydrocyanic acid to the alcohol to the hydrogen chloride to the solvent is 1 (1.1-1.3): (1.4-1.6): (8.5-9.5).
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| CN114181115A (en) * | 2021-12-28 | 2022-03-15 | 山东新和成维生素有限公司 | Salifying system, salifying process and preparation process of trimethyl orthoacetate |
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| CN101619225A (en) * | 2008-06-30 | 2010-01-06 | 汉能科技有限公司 | Reaction kettle for direct coal liquefaction and application thereof |
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