CN216910294U - Perfluoroalkyl alcohol refining plant - Google Patents
Perfluoroalkyl alcohol refining plant Download PDFInfo
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- CN216910294U CN216910294U CN202123431361.6U CN202123431361U CN216910294U CN 216910294 U CN216910294 U CN 216910294U CN 202123431361 U CN202123431361 U CN 202123431361U CN 216910294 U CN216910294 U CN 216910294U
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Abstract
The utility model belongs to the field of mechanical equipment, and particularly relates to a perfluoroalkyl alcohol refining device, which comprises a water feeding system, a reaction system, a water washing system, an alcohol olefin system and a distillation system which are connected through pipelines: the reaction system comprises a reaction kettle; the water washing system comprises a water washing kettle; the distillation device comprises a distillation kettle, a front fraction tank and a positive fraction tank; steam jackets are arranged at the peripheries of the reaction kettle, the washing kettle, the front fraction tank and the positive fraction tank; a heat-conducting oil jacket is arranged at the periphery of the distillation kettle; the discharge end of the water feeding system is communicated with the feed end of the reaction kettle; the feed end of the reaction kettle is communicated with the feed end of the alcohol olefin system; the discharge end of the reaction kettle is communicated with the feed end of the washing kettle; the discharge end of the reaction kettle is communicated with the feed end of the distillation kettle; the discharge end of the distillation kettle is communicated with the feed end of the positive fraction tank and the feed end of the front fraction tank. The refining device has technical superiority in energy consumption, cost, yield, safety and economy, and drives enterprises to develop and improve economic benefits.
Description
Technical Field
The utility model belongs to the field of mechanical equipment, and particularly relates to a perfluoroalkyl alcohol refining device.
Background
The perfluoroalkyl alcohol plays an important role in the organic fluorine chemical industry chain due to the special chemical structure and wide application field. Due to the existence of the perfluorocarbon chain, the perfluoroalkyl alcohol has unique chemical stability, corrosion resistance, flame retardance and hydrophobic and oleophobic properties, and is widely applied to the fields of fabric finishing agents, surfactants, fluorine-containing resins, medical intermediates and the like. Through further functional transformation, the perfluoroalkyl alcohol can be transformed into corresponding thiol, sulfonyl chloride and other various fluorine intermediates, and further used for synthesizing various fluorine-containing surfactants, fluorine-containing fabric finishing agents and other fluorine-containing fine chemicals. Furthermore, perfluoroalkyl alcohols can also be used for the production of synthetic monomers and fluoroethers for fluorine-containing textile finishing agents. China is a world with large fluorite reserves, 1/3 of the reserves accounting for the total reserves of the world is proved, and very favorable conditions are provided for the development of the organic fluorine industry.
At present, the market demand for perfluoroalkyl alcohol is wide in China, but the production technical means of enterprises and units in China according to the process conditions are too traditional, and the operation conditions are very harsh. The production technology of the perfluoroalkyl alcohol is limited in China, so that the raw material market of the perfluoroalkyl alcohol is monopolized by foreign companies for a long time, and meanwhile, the perfluoroalkyl alcohol is converted into fluorine-containing fine chemicals with high added value and high profit to be sold in China.
The perfluoroalkyl alcohol synthetic route in the original industry in China mostly adopts double-layer pipes, and because of more valves, instruments, sight glasses and related pipe fittings on the pipeline, bring certain construction degree of difficulty for the industrial installation on the one hand, increase running cost, on the other hand pipeline dead point is more easily crystallized and causes the pipeline to block up, brings mechanical impurity in the maintenance operation into and influences product quality. In China, a relatively complete preparation method and a refining device are not established for developing the perfluoroalkyl alcohol, so that the productivity is seriously insufficient, and therefore, the development of the process preparation method of the perfluoroalkyl alcohol has important practical significance.
SUMMERY OF THE UTILITY MODEL
In order to overcome the defects of the prior art, the technical problems to be solved by the utility model are as follows: provided is a perfluoroalkyl alcohol refining device which can improve the accuracy and the process safety in the control of the production process.
In order to solve the technical problems, the utility model adopts the technical scheme that: a perfluoroalkyl alcohol refining device comprises a water feeding system, a reaction system, a water washing system, an alcohol olefin system and a distillation system which are connected through pipelines:
the reaction system comprises a reaction kettle; the water washing system comprises a water washing kettle; the distillation device comprises a distillation kettle, a front fraction tank and a positive fraction tank;
steam jackets are arranged at the peripheries of the reaction kettle, the washing kettle, the front fraction tank and the positive fraction tank; a heat-conducting oil jacket is arranged at the periphery of the distillation kettle;
the discharge end of the water feeding system is communicated with the feed end of the reaction kettle; the feed end of the reaction kettle is communicated with the feed end of the alcohol-containing olefin system; the discharge end of the reaction kettle is communicated with the feed end of the washing kettle; the discharge end of the reaction kettle is communicated with the feed end of the distillation kettle; the discharge end of the distillation kettle is communicated with the feed end of the positive fraction tank and the feed end of the front fraction tank.
The reaction system is provided with a steam heat tracing pipe on a pipeline from the raw material to the reaction kettle, and the pipeline from the reaction kettle to the distillation kettle is provided with the steam heat tracing pipe; and the water washing system is provided with a steam heat tracing pipe on a pipeline from the water washing kettle to the reaction kettle.
Wherein, the water feeding system comprises a pure water metering tank; and a water inlet stop valve of the pure water metering tank is arranged on the water inlet pipe of the pure water metering tank.
Wherein, all be equipped with weighing module and teletransmission weighing controller on pure water metering tank, reation kettle, the washing cauldron.
Wherein a first steam inlet pipe and a first steam outlet pipe which are provided with a first steam regulating valve are arranged on a steam jacket of the reaction kettle; the top of the reaction kettle is provided with a plurality of openings, and the plurality of openings of the reaction kettle are respectively provided with a first thermal resistor and a first remote transmission pressure transmitter; the evacuating pipe of the reaction kettle is provided with an evacuating cut-off valve; a feeding stop valve of the reaction kettle is arranged on a feeding pipe of the reaction kettle.
Wherein, a second steam inlet pipe and a second steam outlet pipe which are provided with a second steam regulating valve are arranged on a steam jacket of the water washing kettle; a plurality of openings are formed in the top of the washing kettle, and a second thermal resistor and a second remote transmission pressure transmitter are respectively arranged at the plurality of openings of the washing kettle; a nitrogen pipe of the washing kettle is provided with a nitrogen stop valve; and a water inlet cut-off valve of the washing kettle is arranged on a water inlet pipe of the washing kettle.
Wherein the alcohol olefin system comprises: a reaction condenser and an olefin tank; the alcohol-olefin system is provided with a steam heat tracing pipe on the pipeline from the reaction condenser to the olefin tank and from the olefin tank to the reaction kettle; the reaction condenser comprises a cold brine inlet pipe, a cold brine outlet pipe and a reaction condenser outlet pipe; a third thermal resistor is arranged on an outlet pipe of the reaction condenser; the cold brine inlet pipe and the cold brine outlet pipe are provided with cold brine regulating valves; the olefin tank is arranged on a return pipe between the reaction kettle and the reaction condenser.
Wherein the distillation system further comprises a distillation condenser; and the distillation system is provided with steam tracing pipes on a pipeline from the distillation condenser to the positive fraction tank and an evacuation pipeline of the distillation condenser.
The distillation condenser is provided with a hot water inlet pipe and a hot water outlet pipe which are provided with hot water regulating valves, and a distillation condenser outlet pipe, and the distillation condenser outlet pipe is provided with a fifth thermal resistor.
The heat-conducting oil inlet pipe and the heat-conducting oil outlet pipe with heat-conducting oil regulating valves are arranged on the heat-conducting oil jacket of the distillation kettle; a fourth steam inlet pipe and a fourth steam outlet pipe which are provided with a fourth steam regulating valve are respectively arranged on the steam jacket of the front fraction tank; a third steam inlet pipe and a third steam outlet pipe which are provided with a third steam regulating valve are respectively arranged on the steam jacket of the positive fractionation tank; a fourth thermal resistor is arranged on the heat conduction oil jacket; and a sixth thermal resistor and a seventh thermal resistor are respectively arranged on the steam jackets of the positive fraction tank and the front fraction tank.
The utility model has the beneficial effects that: the utility model provides a preparation method and a refining device of perfluoroalkyl alcohol, which can effectively solve the crystallization defect of products by adopting steam heat tracing, reduce the operation cost and improve the product quality. Secondly, the synthetic process of the refining device is carried out under normal pressure, so that the problems of poor process safety, high equipment cost and the like can be solved. Finally, the automatic control effective investment improves the accuracy and the process safety in the production process control and reduces the labor intensity of workers. In conclusion, the advantages of the technology are reflected in energy consumption, cost, yield, safety and economy.
Drawings
FIG. 1 is a schematic view showing a purification apparatus for a perfluoroalkylethanol according to an embodiment of the present invention;
FIG. 2 is a schematic view showing a water supply system of a perfluoroalkylethanol purification apparatus according to an embodiment of the present invention;
FIG. 3 is a schematic view showing a reaction system of a perfluoroalkylethanol refining apparatus according to an embodiment of the present invention;
FIG. 4 is a schematic view showing a water washing system of a perfluoroalkylethanol refining apparatus according to an embodiment of the present invention;
FIG. 5 is a schematic view showing an alcohol-olefin system of a purification apparatus for a perfluoroalkylethanol according to an embodiment of the present invention;
FIG. 6 is a schematic view showing a distillation system of a purification apparatus for perfluoroalkylethanol according to an embodiment of the present invention;
description of reference numerals:
1. a water delivery system; 101. a pure water metering tank; 102. a water inlet cut-off valve of the pure water metering tank;
2. a reaction system; 201. a reaction kettle; 202. a first thermal resistor; 203. a first steam inlet pipe; 204. a first steam regulating valve; 205. a first vapor outlet pipe; 206. a first remote pressure transmitter; 207. evacuating the shut-off valve; 208. a feeding cut-off valve of the reaction kettle;
3. a water washing system; 301 washing the kettle with water; 302. a second steam regulating valve; 303. a second steam inlet pipe; 304. a second vapor outlet pipe; 305. a second thermal resistor; 306. a second remote pressure transmitter; 307. a nitrogen shut-off valve; 308. a water inlet cut-off valve of the washing kettle;
4. an alcohol with olefin system; 401. a reaction condenser; 402. an olefin tank; 403. cold brine enters the pipe; 404. a cold brine outlet pipe; 405. a condenser outlet pipe; 406. a third thermal resistance; 407. a cold brine regulating valve;
5. a distillation system; 501. a distillation kettle; 502. a positive distillation tank; 503. a front cut tank; 504. a distillation condenser; 505. a heat conducting oil regulating valve; 506. a heat conducting oil inlet pipe; 507. a heat conducting oil outlet pipe; 508. a third steam regulating valve; 509. a third steam inlet pipe; 510. a third vapor outlet pipe; 511. a fourth steam regulating valve; 512. a fourth steam inlet pipe; 513. a fourth vapor outlet pipe; 514. a fourth thermal resistance; 515. a hot water regulating valve; 516. a hot water inlet pipe; 517. a hot water outlet pipe; 518. a fifth thermal resistor; 519. a sixth thermal resistance; 520. and a seventh thermal resistance.
Detailed Description
In order to explain technical contents, achieved objects, and effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments.
The most key concept of the utility model is as follows: the provided perfluoroalkyl alcohol refining device improves the accuracy and the process safety in the control of the production process.
Referring to fig. 1 to 6, the apparatus for purifying perfluoroalkylethanol of the present invention comprises a water feeding system 1, a reaction system 2, a water washing system 3, an alcohol-olefin-carrying system 4, and a distillation system 5:
the reaction system 2 comprises a reaction kettle 201; the water washing system 3 comprises a water washing kettle 301; the distillation device comprises a distillation kettle 501, a positive fraction tank 502 and a front fraction tank 503;
steam jackets are arranged on the peripheries of the reaction kettle 201, the washing kettle 301, the positive fraction tank 502 and the front fraction tank 503; a heat conducting oil jacket is arranged on the periphery of the distillation kettle 501;
the discharge end of the water feeding system 1 is communicated with the feed end of the reaction kettle 201; the feed end of the reaction kettle 201 is communicated with the feed end of the alcohol olefin-carrying system 4; the discharge end of the reaction kettle 201 is communicated with the feed end of the water washing kettle 301; the discharge end of the reaction kettle 201 is communicated with the feed end of the distillation kettle 501; the discharge end of the distillation kettle 501 is communicated with the feed end of the positive fraction tank 502 and the feed end of the front fraction tank 503.
From the above description, the beneficial effects of the present invention are: the utility model provides a perfluoroalkyl alcohol refining device, which has less use than the existing perfluoroalkyl alcohol refining device (adopting a double-layer pipe) and accessories such as valves, instruments, sight glasses and the like, is simple to install and construct and is convenient to maintain; by arranging the water feeding system, the reaction system, the water washing system, the alcohol olefin system and the distillation system, and communicating the reaction system with the alcohol olefin system, the problems of greatly reduced yield and increased energy consumption caused by the extraction of reactants and perfluoroalkyl alcohol due to overhigh kettle temperature are effectively avoided; different jacket structures are configured according to the requirements of different system preparation for heating, the temperature can be accurately controlled and adjusted, and the influence of unstable temperature of the traditional heating mode on the product purity and yield is avoided. The perfluoroalkyl alcohol is prepared by using the perfluoroalkyl alcohol process refining device without using strong acidic media such as concentrated sulfuric acid, nitric acid and the like, thereby effectively solving the problems of poor process safety and the like.
Further, in the reaction system 2, a steam heat tracing pipe is arranged on a pipeline from the raw material to the reaction kettle 201, and a steam heat tracing pipe is arranged on a pipeline from the reaction kettle 201 to the distillation kettle 501; the water washing system 3 is provided with a steam heat tracing pipe on a pipeline from the water washing kettle 301 to the reaction kettle 201; the distillation system 5 is provided with a steam tracing pipe on a pipeline from the distillation condenser to the positive distillate tank 502.
From the above description, can effectively solve the drawback of product crystallization in the pipeline transportation process through setting up steam heat tracing pipe, reduce the running cost, promote product quality. And the problems that the pipeline is required to be frequently stopped for maintenance and repair and the production efficiency is influenced due to the fact that the pipeline is blocked because the dead points of the pipeline are easy to crystallize are avoided.
Further, the water supply system 1 includes a pure water metering tank 101; the water inlet pipe of the pure water metering tank 101 is provided with a pure water metering tank water inlet cut-off valve 102.
Further, an air respirator is arranged at the top of the pure water metering tank 101. The air respirator is used to discharge air from the pure water tank 101.
According to the above description, the pure water metering tank weight and the water inlet cut-off valve in the feeding system are interlocked to realize automatic control of the water inlet weight of the pure water metering tank, meanwhile, a high limit alarm is set for the pure water metering tank weight, when the pure water metering tank weight reaches a high limit value, the automatic control system makes a corresponding sound alarm indication, the phenomenon that the pure water metering tank overflows into the air respirator is avoided, and automatic, safe, stable and accurate metering of pure water is realized.
Furthermore, the pure water metering tank 101, the reaction kettle 201 and the water washing kettle 301 are provided with a weighing module and a remote weighing controller.
Further, the weighing modules are arranged in the middle of the pure water metering tank 101, the reaction kettle 201 and the washing kettle 301, and the number of the weighing modules can be four.
According to the description, the weighing module and the remote weighing controller are used for weighing the weights of the pure water metering tank, the reaction kettle and the washing kettle, so that the weight of each container is effectively regulated and controlled, and accurate feeding metering is realized. The feeding weight is automatically controlled by interlocking with a cut-off valve.
Further, a first steam inlet pipe 203 and a first steam outlet pipe 205 which are provided with a first steam regulating valve 204 are arranged on a steam jacket of the reaction kettle 201; a plurality of openings are formed in the top of the reaction kettle 201, and a first thermal resistor 202 and a first remote transmission pressure transmitter 206 are respectively arranged at the plurality of openings; an evacuation shut-off valve 207 is arranged on an evacuation pipe of the reaction kettle 201; a feed pipe of the reaction kettle 201 is provided with a reaction kettle feed cut-off valve 208.
Further, a threaded connection is adopted between the first thermal resistor 202 and the opening of the reaction kettle 201.
From the above description, reation kettle weight among the reaction system and reation kettle feeding trip valve interlocking realize the automatic control of reation kettle feeding weight, effectively solve evacuation of reation kettle and run the material and accurate feeding measurement problem to set up the high limit warning to reation kettle weight, when reation kettle feeding volume reaches the high limit value, the system reports to the police and reminds the operator, prevents to bring the potential safety hazard in a certain extent for follow-up reaction because of manual feeding volume too big messenger gas phase space.
Further, a second steam inlet pipe 303 and a second steam outlet pipe 304 which are provided with a second steam regulating valve 302 are arranged on a steam jacket of the water washing kettle 301; a plurality of openings are formed in the top of the washing kettle 301, and a second thermal resistor 305 and a second remote transmission pressure transmitter 305 are respectively arranged at the plurality of openings; a nitrogen pipe of the water washing kettle 301 is provided with a nitrogen stop valve 306; the inlet pipe of the water washing kettle 301 is provided with a water inlet cut-off valve 307 of the water washing kettle.
As can be seen from the above description, the second steam regulating valve in the water washing system is used for controlling the second steam inlet pipe to supply steam into the steam jacket of the water washing kettle, so as to regulate the temperature of the water washing kettle. The automatic control of washing temperature is realized to washing cauldron temperature and second steam control valve interlocking, solves the accurate measurement and the control water material ratio that pure water intake on the one hand, and the accurate accuse temperature of on the other hand can stop the insufficient problem of washing that the product crystallization caused, and the poor problem of process safety nature that washing cauldron superpressure brought can be avoided in automatic pressure rise, and effective accuse simultaneously presses the input cost that can reduce equipment.
Further, the alcohol olefin-bearing system 4 includes: a reaction condenser 401 and an olefin tank 402; the alcohol olefin-carrying system 4 is additionally provided with a steam heat tracing pipe on the pipelines from the reaction condenser 401 to the olefin tank 402 and from the olefin tank 402 to the reaction kettle 201; the reaction condenser 401 comprises a cold brine inlet pipe 403, a cold brine outlet pipe 404 and a reaction condenser outlet pipe 405; a third thermal resistor 406 is arranged on the outlet pipe 405 of the reaction condenser; a cold brine regulating valve 407 is arranged on the cold brine inlet pipe 403 and the cold brine outlet pipe 404; the olefin tank 402 is disposed on the return pipe of the reaction kettle 201.
From the above description, the outlet temperature of the reaction condenser in the system for carrying the perfluoroalkyl alcohol by the alcohol and the reaction cold brine regulating valve are interlocked to realize the automatic control of the outlet temperature of the reaction condenser, so that on one hand, the perfluoroalkyl alcohol is prevented from being carried out due to overhigh kettle temperature, thereby greatly reducing the yield, and on the other hand, the cold brine amount is controlled to prevent the methanol volatilization from influencing the carrying-out amount and carrying-out efficiency of the byproduct olefin, thereby reducing the purity of the perfluoroalkyl alcohol and increasing the energy consumption.
Further, the distillation system 5 further comprises a distillation condenser 504; the distillation system 5 is provided with steam tracing pipes on a pipeline from the distillation condenser 504 to the positive fraction tank 502 and an evacuation pipeline of the distillation condenser 504.
From the above description, the adoption of steam heat tracing can effectively solve the crystallization defect of the product, reduce the operation cost and improve the product quality.
Furthermore, the distillation condenser 504 is provided with a hot water inlet pipe 516 and a hot water outlet pipe 517 with a hot water regulating valve 515, and a distillation condenser outlet pipe, and the distillation condenser outlet pipe is provided with a fifth thermal resistor 518.
From the description above, the addition of the hot water inlet pipe and the hot water outlet pipe can ensure that the material is supercooled, cooled and crystallized in the process control, so that the pipeline is blocked to influence extraction, and can avoid material loss caused by extraction of overheated material along with evacuation; the addition of the heat conducting oil can accurately control and adjust the temperature in the distillation kettle, thereby avoiding the influence on the product yield caused by abnormal change of fractions due to unstable temperature rise.
Further, a heat conduction oil inlet pipe 506 and a heat conduction oil outlet pipe 507 with a heat conduction oil regulating valve 505 are arranged on a heat conduction oil jacket of the distillation kettle 501; a third steam inlet pipe 509 and a third steam outlet pipe 510 which are provided with a third steam regulating valve 508 are respectively arranged on the steam jacket of the positive fraction tank 502; a fourth steam inlet pipe 512 and a fourth steam outlet pipe 513 with a fourth steam regulating valve 511 are respectively arranged on the steam jacket of the front fractionating tank 503; a fourth thermal resistor 514 is arranged on the heat conducting oil jacket; a hot water inlet pipe 516 and a hot water outlet pipe 517 with a hot water regulating valve 515 are arranged on the distillation condenser 504, and a fifth thermal resistor 518 is arranged on an outlet pipe of the distillation condenser 504; a sixth thermal resistor 519 and a seventh thermal resistor 520 are respectively arranged on the steam jackets of the positive distillate tank 502 and the front distillate tank 503.
Furthermore, the sixth thermal resistor 519 is in threaded connection with the lower head pipe orifice of the positive fraction tank 502, and the seventh thermal resistor 520 is in threaded connection with the lower head pipe orifice of the front fraction tank 503.
As can be seen from the above description, the interlocking of the positive fraction tank temperature and the positive fraction tank steam regulating valve in the distillation system realizes the automatic control of the positive fraction tank temperature. And opening a heat conduction oil regulating valve of the distillation kettle, supplying heat conduction oil to the distillation kettle, timely switching the rectification tank according to the tower top temperature of the rectification tower and the outlet temperature of the distillation condenser, and regulating the opening degree of the hot water regulating valve. And (3) after the temperature of the distillation kettle reaches the set temperature and the extraction sight glass does not extract materials, finishing distillation, and filling the perfluoroalkyl alcohol finished product in the positive distillation tank. The hot water pipe is additionally arranged, so that on one hand, the influence of blocking a pipeline due to supercooling of materials in process control and cooling crystallization can be ensured, and on the other hand, the material loss caused by the fact that overheated materials are brought out along with evacuation can be avoided; the heat conducting oil inlet and outlet pipe is additionally arranged, so that the temperature in the distillation kettle can be accurately controlled and adjusted, and the influence on the product yield caused by abnormal change of fractions due to unstable temperature rise is avoided.
Application scenarios: the refining device is applied to the industrial preparation of perfluoroalkyl alcohol.
Referring to fig. 1 to 6, a first embodiment of the present invention is: the refining device of perfluoroalkyl alcohol is a refining device with automatic water feeding, cutting off interlocking, reaction pumping, cutting off interlocking, reaction heating regulation interlocking, water washing heating regulation interlocking, material beating, pressure supplementing, cutting off interlocking, condensation temperature control regulation interlocking, distillation heating regulation interlocking and collection heat preservation regulation interlocking, and comprises a water feeding system, a reaction system, a water washing system, an alcohol belt olefin system and a distillation system:
the water feeding system 1 comprises a pure water metering tank 101; the water inlet pipe of the pure water metering tank 101 is provided with a pure water metering tank water inlet cut-off valve 102. The middle part of the pure water metering tank 101 is provided with 4 weighing modules and a remote weighing controller.
The reaction system 2 comprises a reaction kettle 201; a first steam inlet pipe 203 and a first steam outlet pipe 205 which are provided with a first steam regulating valve 204 are arranged on a steam jacket of the reaction kettle 201; a plurality of openings are formed in the top of the reaction kettle 201, and a first thermal resistor 202 and a first remote transmission pressure transmitter 206 are respectively arranged at the plurality of openings; an evacuation shut-off valve 207 is arranged on an evacuation pipe of the reaction kettle 201; a feed pipe of the reaction kettle 201 is provided with a reaction kettle feed cut-off valve 208. The middle part of the reaction kettle 201 is provided with 4 weighing modules and a remote weighing controller.
The water washing system 3 comprises a water washing kettle 301; a second steam inlet pipe 303 and a second steam outlet pipe 304 which are provided with a second steam regulating valve 302 are arranged on a steam jacket of the water washing kettle 301; a plurality of openings are formed in the top of the washing kettle 301, and a second thermal resistor 305 and a second remote transmission pressure transmitter 305 are respectively arranged at the plurality of openings; a nitrogen pipe of the water washing kettle 301 is provided with a nitrogen stop valve 306; and a water inlet stop valve 307 of the water washing kettle is arranged on the water inlet pipe of the water washing kettle 301. The middle part of the water washing kettle 301 is provided with 4 weighing modules and a remote weighing controller.
The alcohol olefin-bearing system 4 includes: a reaction condenser 401 and an olefin tank 402; the alcohol olefin-carrying system 4 is additionally provided with a steam heat tracing pipe on the pipelines from the reaction condenser 401 to the olefin tank 402 and from the olefin tank 402 to the reaction kettle 201; the reaction condenser 401 comprises a cold brine inlet pipe 403, a cold brine outlet pipe 404 and a reaction condenser outlet pipe 405; a third thermal resistor 406 is arranged on the outlet pipe 405 of the reaction condenser; a cold brine regulating valve 407 is arranged on the cold brine inlet pipe 403 and the cold brine outlet pipe 404; the olefin tank 402 is disposed on the return pipe of the reaction kettle 201.
The distillation device comprises a distillation kettle 501, a positive fraction tank 502, a front fraction tank 503 and a distillation condenser 504; steam jackets are arranged on the peripheries of the reaction kettle 201, the washing kettle 301, the positive fraction tank 502 and the front fraction tank 503; and a heat conduction oil jacket is arranged on the periphery of the distillation kettle 501.
A steam heat tracing pipe is additionally arranged on an outlet pipeline of the distillation condenser 504; a heat conduction oil inlet pipe 506 and a heat conduction oil outlet pipe 507 with a heat conduction oil regulating valve 505 are arranged on a heat conduction oil jacket of the distillation kettle 501; a third steam inlet pipe 509 and a third steam outlet pipe 510 which are provided with a third steam regulating valve 508 are respectively arranged on the steam jacket of the positive fraction tank 502; a fourth steam inlet pipe 512 and a fourth steam outlet pipe 513 which are provided with a fourth steam regulating valve 511 are respectively arranged on the steam jacket of the front fraction tank 503; a fourth thermal resistor 514 is arranged on the heat conducting oil jacket; a hot water inlet pipe 516 and a hot water outlet pipe 517 with a hot water regulating valve 515 are arranged on the distillation condenser 504, and a fifth thermal resistor 518 is arranged on an outlet pipe of the distillation condenser 504; a sixth thermal resistor 519 and a seventh thermal resistor 520 are respectively arranged on the steam jackets of the positive distillate tank 502 and the front distillate tank 503.
The discharge end of the water feeding system 1 is communicated with the feed end of the reaction kettle 201; the feed end of the reaction kettle 201 is communicated with the feed end of the alcohol olefin-carrying system 4; the discharge end of the reaction kettle 201 is communicated with the feed end of the water washing kettle 301; the discharge end of the reaction kettle 201 is communicated with the feed end of the distillation kettle 501; the discharge end of the distillation kettle 501 is communicated with the feed end of the positive fraction tank 502 and the feed end of the front fraction tank 503.
The reaction system 2 is provided with a steam heat tracing pipe on a pipeline from the raw material to the reaction kettle 201, and is provided with a steam heat tracing pipe on a pipeline from the reaction kettle 201 to the distillation kettle 501; the water washing system 3 is provided with a steam heat tracing pipe on a pipeline from the water washing kettle 301 to the reaction kettle 201; the distillation system 5 is provided with a steam tracing pipe on a pipeline from the distillation condenser to the positive distillate tank 502.
The working process of the utility model is as follows: the water delivery system is provided with the pure water metering tank, and the top of the pure water metering tank is provided with the air respirator. The air respirator is used for exhausting the air in the pure water metering tank. The pure water metering tank is provided with an air respirator, and when the pure water metering tank is in a water inlet state, a cut-off valve for water inlet of the pure water metering tank can be opened. The pure water metering tank is provided with a weighing module and a remote weighing controller for weighing. And after the weight of the pure water metering tank reaches the set weight, automatically closing the stop valve for water inlet of the pure water metering tank. The pure water metering tank and the water inlet cut-off valve are interlocked to realize automatic control of the water inlet weight of the pure water metering tank, and meanwhile, a high limit alarm is set for the weight of the pure water metering tank. When the weight of the pure water metering tank reaches a high limit value, the automatic control system makes corresponding sound and report instructions.
When the reaction kettle in the reaction system is in a feeding state, the evacuation stop valve is opened. The second remote pressure transmitter is used for measuring the pressure of the system. And after the pressure in the reaction kettle reaches the set pressure, automatically closing the evacuation stop valve. The pressure of the reaction kettle is interlocked with the evacuation stop valve to realize the automatic control of the material pumping pressure of the reaction kettle. And opening a feed cut-off valve of the reaction kettle, and starting to supply raw materials to the reaction kettle through a pipeline by the pure water metering tank. The reaction kettle is provided with a weighing module and a remote weighing controller for weighing. And after the weight of the reaction kettle reaches the set weight, automatically closing the feed cut-off valve of the reaction kettle. The automatic control of reation kettle feeding weight is realized to reation kettle and feeding trip valve interlocking to set up the high limit to the reation kettle weight and report to the police, when reation kettle feeding volume reached the high limit value, the system reported to the police and reminded the operator.
When the feeding is finished and the reaction kettle has a temperature rise condition, the reaction condenser of the alcohol and olefin system can be opened, the first steam regulating valve is opened, and steam is supplied to the reaction kettle. The first thermal resistor is used for temperature measurement of the system. And after the temperature of the materials in the reaction kettle reaches the set temperature, automatically adjusting the opening size of the first steam adjusting valve to maintain the temperature of the reaction kettle within the set temperature range, and cooling the reaction liquid through the reaction condenser and refluxing the reaction liquid into the reaction kettle. The reaction kettle and the first steam regulating valve are interlocked to realize the automatic control of the reaction temperature of the reaction kettle.
When the reaction is finished and the washing kettle has the washing condition, a water inlet cut-off valve of the washing kettle of the washing system can be opened to supply pure water to the washing kettle. The washing kettle is provided with a weighing module and a remote weighing controller for weighing. And after the weight of the washing kettle reaches the set weight, automatically closing the water inlet stop valve of the washing kettle. The water washing kettle and the water inlet cut-off valve are interlocked to realize automatic control of the water inlet weight of the water washing kettle. And opening a second steam regulating valve to supply steam to the water washing kettle, wherein a second thermal resistor is used for measuring the temperature of the system. And after the temperature of the pure water in the washing kettle reaches the set temperature, automatically adjusting the opening size of the second steam regulating valve to maintain the temperature of the washing kettle in the set temperature range, opening relevant valves between the reaction kettle and a washing kettle pipeline to enable reaction liquid to enter the washing kettle, and interlocking the washing kettle and the second steam regulating valve to realize the automatic control of the washing temperature. After the water washing and standing are finished, the nitrogen stop valve is opened, the water washing kettle is pressurized, and the second remote transmission pressure transmitter is used for measuring the pressure of the system. And after the pressure in the washing kettle reaches a set pressure, automatically cutting off the nitrogen stop valve, opening a relevant valve on the balance pipe, pumping the washed lower-layer organic phase into the reaction kettle through the balance pipe, and conveying the upper-layer washing liquid to a sedimentation tank. The washing kettle and the nitrogen stop valve are interlocked to realize the automatic control of the material beating pressure of the washing kettle.
When the material beating is finished and the reaction kettle has the condition of alcohol with olefin, methanol with set weight is added into the reaction kettle, a cold brine regulating valve at minus 5 ℃ on a reaction condenser is opened, cold brine at minus 5 ℃ is supplied to the reaction condenser, a steam regulating valve of the reaction kettle is opened, steam is supplied to the reaction kettle, the opening of the steam regulating valve of the reaction kettle is automatically adjusted after the temperature of materials in the reaction kettle reaches the set temperature, the methanol is cooled by the reaction condenser and flows back into the reaction kettle through an olefin tank, and the opening of the cold brine regulating valve is automatically adjusted after the temperature of the top of the reaction condenser reaches the set temperature, so that the methanol is completely condensed and flows back into the reaction kettle. The reaction condenser and the cold brine regulating valve are interlocked to realize the automatic control of the outlet temperature of the reaction condenser.
When the distillation kettle is in a feeding state, the material with olefin through alcohol is placed into the distillation kettle, related valves evacuated by a distillation system can be opened, hot water inlet and outlet pipes of a distillation condenser are opened, a hot water adjusting valve on a shell layer of the distillation condenser is opened to supply hot water to the distillation condenser, a steam adjusting valve on a front fraction groove jacket can be opened respectively to supply steam to the front fraction groove. The fourth thermal resistor is used for measuring the temperature in the distillation kettle, and the fifth thermal resistor is used for measuring the temperature at the outlet of the distillation condenser. And after the temperature in the front fraction tank reaches the set temperature, automatically adjusting the opening of the steam regulating valve of the front fraction tank to maintain the temperature in the front fraction tank within the set temperature range, and interlocking the front fraction tank and the steam regulating valve of the front fraction tank to realize the automatic control of the temperature of the front fraction tank. And opening a heat conduction oil regulating valve of the distillation kettle to supply heat conduction oil to the distillation kettle. The sixth thermal resistor is used for measuring the temperature of the front fraction tank, and the seventh thermal resistor is used for measuring the temperature of the front fraction tank. And after the temperature in the distillation kettle reaches the set temperature, slowly adjusting the opening of a heat conduction oil adjusting valve of the distillation kettle to maintain the temperature in the distillation kettle in the set temperature range, timely switching a front fraction tank and adjusting the opening of a hot water adjusting valve according to the temperature at the top of the rectifying tower and the outlet temperature of a distillation condenser, and after the temperature of the distillation kettle reaches the set temperature and no material is extracted from an extraction view mirror, finishing distillation and filling a perfluoroalkyl alcohol finished product in a front fraction tank.
In conclusion, the utility model provides a perfluoroalkyl alcohol refining device, which is used for promoting and optimizing a perfluoroalkyl alcohol process refining device, and effectively solves the problems of evacuation and material running of a reaction kettle and accurate feeding and metering by automatically controlling the feeding weight of the reaction kettle; the automatic control of the reaction temperature of the reaction kettle is realized, the problem of unstable control of the reaction temperature caused by manual operation of a steam hand valve is effectively solved, the normal reflux of the reaction is influenced, and the reaction cannot be fully carried out; according to the utility model, on one hand, the accurate metering of pure water inlet and the control of water-material ratio are solved, on the other hand, the accurate temperature control can prevent the problem of insufficient water washing caused by product crystallization, the automatic pressure rise can avoid the problem of poor process safety caused by overpressure of a water washing kettle, and meanwhile, the effective pressure control can reduce the investment cost of equipment; the automatic control of the outlet temperature of the reaction condenser is realized, thereby preventing perfluoroalkyl alcohol from being brought out due to overhigh kettle temperature, greatly reducing the yield, and controlling the cold salt water amount to prevent methanol volatilization from influencing the bringing-out amount and the bringing-out efficiency of byproduct olefin, thereby reducing the purity of perfluoroalkyl alcohol and increasing the energy consumption.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to the related technical fields, are included in the scope of the present invention.
Claims (10)
1. The perfluoroalkyl alcohol refining device is characterized by comprising a water feeding system, a reaction system, a water washing system, an alcohol olefin-carrying system and a distillation system which are connected through pipelines:
the reaction system comprises a reaction kettle;
the water washing system comprises a water washing kettle;
the distillation system comprises a distillation kettle, a front fraction tank and a positive fraction tank;
steam jackets are arranged at the peripheries of the reaction kettle, the washing kettle, the front fraction tank and the positive fraction tank; a heat-conducting oil jacket is arranged at the periphery of the distillation kettle;
the discharge end of the water feeding system is communicated with the feed end of the reaction kettle;
the feed end of the reaction kettle is communicated with the feed end of the alcohol-containing olefin system;
the discharge end of the reaction kettle is communicated with the feed end of the washing kettle;
the discharge end of the reaction kettle is communicated with the feed end of the distillation kettle;
the discharge end of the distillation kettle is communicated with the feed end of the positive fraction tank and the feed end of the front fraction tank.
2. The refining device of perfluoroalkyl alcohol according to claim 1, characterized in that the reaction system is provided with a steam heat tracing pipe on the pipeline from the raw material to the reaction kettle, and a steam heat tracing pipe on the pipeline from the reaction kettle to the distillation kettle;
and the water washing system is provided with a steam heat tracing pipe on a pipeline from the water washing kettle to the reaction kettle.
3. A perfluoroalkyl alcohol refining device according to claim 1, characterized in that said water supply system comprises a pure water metering tank; and a water inlet stop valve of the pure water metering tank is arranged on the water inlet pipe of the pure water metering tank.
4. The refining device of perfluoroalkyl alcohol according to claim 3, wherein the pure water metering tank, the reaction kettle, and the washing kettle are equipped with weighing modules and remote weighing controllers.
5. The refining device of perfluoroalkyl alcohol according to claim 1, characterized in that the steam jacket of the reaction kettle is provided with a first steam inlet pipe and a first steam outlet pipe with a first steam regulating valve;
a plurality of openings are formed in the top of the reaction kettle, and a first thermal resistor and a first remote transmission pressure transmitter are respectively arranged at the plurality of openings of the reaction kettle; the evacuating pipe of the reaction kettle is provided with an evacuating cut-off valve; a feeding stop valve of the reaction kettle is arranged on a feeding pipe of the reaction kettle.
6. The refining device of perfluoroalkyl alcohol according to claim 1, characterized in that the steam jacket of the water washing kettle is provided with a second steam inlet pipe and a second steam outlet pipe having a second steam regulating valve;
a plurality of openings are formed in the top of the washing kettle, and a second thermal resistor and a second remote transmission pressure transmitter are respectively arranged at the plurality of openings of the washing kettle; a nitrogen pipe of the washing kettle is provided with a nitrogen stop valve; and a water inlet cut-off valve of the washing kettle is arranged on a water inlet pipe of the washing kettle.
7. A perfluoroalkyl alcohol refining device according to claim 1, characterized in that said alcohol-carrying olefin system comprises: a reaction condenser and an olefin tank;
the alcohol-olefin system is provided with a steam heat tracing pipe on the pipeline from the reaction condenser to the olefin tank and from the olefin tank to the reaction kettle;
the reaction condenser comprises a cold brine inlet pipe, a cold brine outlet pipe and a reaction condenser outlet pipe; a third thermal resistor is arranged on an outlet pipe of the reaction condenser; the cold brine inlet pipe and the cold brine outlet pipe are provided with cold brine regulating valves;
the olefin tank is arranged on a return pipe between the reaction kettle and the reaction condenser.
8. The apparatus for refining perfluoroalkylethanol as recited in claim 1, wherein said distillation system further comprises a distillation condenser;
and the distillation system is provided with steam tracing pipes on a pipeline from the distillation condenser to the positive fraction tank and an evacuation pipeline of the distillation condenser.
9. A perfluoroalkyl alcohol refining plant as claimed in claim 8, characterized in that said distillation condenser is provided with a hot water inlet pipe and a hot water outlet pipe having hot water regulating valves, and a distillation condenser outlet pipe, said distillation condenser outlet pipe being provided with a fifth thermal resistor.
10. The refining device of perfluoroalkyl alcohol according to claim 1, characterized in that a heat transfer oil inlet pipe and a heat transfer oil outlet pipe with a heat transfer oil regulating valve are arranged on the heat transfer oil jacket of the distillation still;
a fourth steam inlet pipe and a fourth steam outlet pipe which are provided with a fourth steam regulating valve are respectively arranged on the steam jacket of the front fraction tank;
a third steam inlet pipe and a third steam outlet pipe which are provided with a third steam regulating valve are respectively arranged on the steam jacket of the positive fractionation tank;
a fourth thermal resistor is arranged on the heat conduction oil jacket;
and a sixth thermal resistor and a seventh thermal resistor are respectively arranged on the steam jackets of the positive fraction tank and the front fraction tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123431361.6U CN216910294U (en) | 2021-12-30 | 2021-12-30 | Perfluoroalkyl alcohol refining plant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123431361.6U CN216910294U (en) | 2021-12-30 | 2021-12-30 | Perfluoroalkyl alcohol refining plant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216910294U true CN216910294U (en) | 2022-07-08 |
Family
ID=82257035
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202123431361.6U Active CN216910294U (en) | 2021-12-30 | 2021-12-30 | Perfluoroalkyl alcohol refining plant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN216910294U (en) |
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2021
- 2021-12-30 CN CN202123431361.6U patent/CN216910294U/en active Active
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Denomination of utility model: A Refining Device for Perfluoroalkyl Ethanol Effective date of registration: 20230925 Granted publication date: 20220708 Pledgee: Industrial and Commercial Bank of China Limited Sanming Sanyuan Branch Pledgor: FUJIAN SANNONG NEW MATERIALS CO.,LTD. Registration number: Y2023980058306 |