CN118461022B - Perfluoro tripropylamine electrolytic tank capable of detecting liquid density - Google Patents

Abstract

The present invention discloses a perfluorotripropylamine electrolytic cell capable of detecting liquid density, comprising: an electrolytic cell body; a refrigeration heat exchanger, comprising a vertical heat exchange tank, the upper and lower sides of the vertical heat exchange tank are respectively fixedly connected with corresponding upper and lower partitions, and a plurality of corresponding heat exchange circulation pipes are connected through the upper and lower partitions; a heat exchange medium circulation mechanism, comprising a heat exchange jacket fixedly connected to the outer side of the vertical heat exchange tank on the lower side of the lower partition in a sandwich state; a multifunctional isolation mechanism, comprising a movable isolation member arranged in the vertical heat exchange tank on the lower side of the circulating feed pipe; an isolation member driving mechanism, comprising a driving hydraulic cylinder arranged on the bottom side of the heat exchange jacket, the piston rod of the driving hydraulic cylinder is retracted to drive the movable isolation member to squeeze and output the product stored on its bottom side from the product discharge pipe. The present invention can effectively and conveniently output the product, and can significantly reduce the entrainment of the electrolytic mother liquor when the product is output.

Description

A perfluorotripropylamine electrolytic cell capable of detecting liquid density

Technical Field

The invention relates to the technical field of equipment for preparing perfluorotripropylamine, in particular to a perfluorotripropylamine electrolytic cell capable of detecting liquid density.

Background Art

Perfluorotripropylamine is completely non-toxic to the human body and can dissolve and carry a large amount of oxygen and carbon dioxide. It is one of the main components of artificial plasma used in modern medicine. It is also used as an anti-corrosion transmission fluid, dielectric insulation fluid, and leak detection fluid for electronic components and devices. Therefore, the production of perfluorotripropylamine is of great significance to scientific progress and development.

The most widely used technology for preparing perfluorotripropylamine is the electrolytic fluorination method. A mother liquor composed of tripropylamine and hydrogen fluoride is passed through a low-voltage direct current in an electrolytic cell to generate free fluorine atoms to directly replace the hydrogen atoms in tripropylamine. After a simple purification treatment, the perfluorotripropylamine product can be obtained. In this process, it is necessary to circulate the mother liquor and the product through a corresponding refrigeration heat exchanger to cool the mother liquor and the product, so as to prevent the mother liquor and the product from gasifying due to temperature rise during the electrolysis process. Since the density of the electrolytic product "perfluorotripropylamine" is higher than that of the mother liquor, there will be obvious stratification between the prepared product and the mother liquor. At present, the method for collecting the product after the electrolytic cell is completed is mainly to output the material located at the bottom side of the electrolytic cell. Since the mother liquor in the electrolysis process needs to circulate through the refrigeration heat exchanger, the material in the electrolytic cell has continuous fluctuations, resulting in a large amount of mother liquor entrainment in the output product, which is very troublesome. In order to solve the above problem, the existing practice is to stop the machine to output the product, and then re-enter the electrolysis operation after the product output is completed. This will undoubtedly greatly reduce the production efficiency of the product.

Therefore, the research purpose of the present invention is to design a perfluorotripropylamine electrolytic cell that can detect liquid density and can output the product effectively and conveniently without stopping the machine, that is, without affecting the electrolysis process, and can significantly reduce the amount of entrainment of the electrolytic mother liquor during product output.

Summary of the invention

In view of the technical problems existing in the above-mentioned prior art, the present invention provides a perfluorotripropylamine electrolytic cell capable of detecting liquid density, which can effectively solve the technical problems existing in the above-mentioned prior art.

The technical solution of the present invention is:

A perfluorotripropylamine electrolytic cell capable of detecting liquid density, comprising:

An electrolytic cell body, one side of which is provided with a mother liquid inlet pipe, and the electrolytic cell body 1 is an existing electrolytic cell, which is an existing device, and its specific structure is not described here;

A refrigeration heat exchanger, comprising a vertical heat exchange tank, wherein the upper and lower sides of the vertical heat exchange tank are respectively fixedly connected with corresponding upper partitions and lower partitions, and a plurality of corresponding heat exchange circulation pipes are connected through the upper and lower partitions, the vertical heat exchange tank on the bottom side of the lower partition is connected to the bottom of the electrolytic cell body through a corresponding circulation feed pipe pump, the vertical heat exchange tank on the upper side of the upper partition is connected to the upper part of the electrolytic cell body through a corresponding circulation return pipe, and the bottom end of the vertical heat exchange tank is connected to the corresponding product discharge pipe through a corresponding one-way valve;

The heat exchange medium circulation mechanism comprises a heat exchange jacket fixedly connected to the outer side of the vertical heat exchange tank on the lower side of the lower partition in a sandwich state, a conducting pipe connected to the vertical heat exchange tank on the upper side of the lower partition is arranged on the upper part of the heat exchange jacket, a refrigerant inlet pipe is connected to the bottom side of the heat exchange jacket, and a refrigerant discharge pipe is connected to the vertical heat exchange tank on the lower side of the upper partition;

The multifunctional isolating mechanism comprises a movable isolating member arranged in the vertical heat exchange tank at the lower side of the circulating feed pipe, a retractable bellows is connected downwardly to the middle part of the movable isolating member, a corresponding limit tube is installed between the vertical heat exchange tank and the bottom of the heat exchange jacket, the bottom side of the retractable bellows is sleeved in the limit tube, and the bottom end of the retractable bellows is sealed and connected to the bottom of the heat exchange jacket; a plurality of corresponding mounting holes are arranged in an annular array on the movable isolating member, a plurality of corresponding liquid permeable holes are arranged around the mounting holes, and plugging members with an I-shaped cross section can be lifted and installed at the mounting holes, the density of the plugging member is less than the density of the product and greater than the density of the mother liquid, the bottom of the plugging member can form a blockage for the liquid permeable hole, and the top of the plugging member does not form a blockage for the liquid permeable hole;

The isolation member driving mechanism comprises a driving hydraulic cylinder arranged on the bottom side of the heat exchange jacket, the piston rod end of the driving hydraulic cylinder is sleeved in the retractable bellows and connected to the bottom side of the movable isolation member, and at least one corresponding pressure sensor is arranged on the movable isolation member, and one of the sealing members floats up to the position to form abutment and compression against the pressure sensor. When the height of the product stored at the bottom of the vertical heat exchange tank rises to the height of the top of the sealing member, the force exerted by the sealing member on the pressure sensor under the action of its maximum buoyancy reaches a set value, and the piston rod of the driving hydraulic cylinder retracts to drive the movable isolation member to extrude and output the product stored on its bottom side from the product discharge pipe.

The movable isolating member is evenly filled with a plurality of corresponding vibration-reducing damping particles.

A corresponding siphon tee is connected to the product discharge pipe outside the one-way valve, and the siphon section of the siphon tee is connected to the bottom interval between the telescopic bellows and the limiting pipe.

The signal line of the pressure sensor passes through the retractable bellows and is connected to an external electrical controller.

The product discharge pipe is connected to the corresponding intermediate tank.

The intermediate tank pump is connected to the feed end of the corresponding distillation equipment.

The upper right side of the electrolytic cell body is externally connected with a tail gas exhaust pipe.

The left side of the electrolytic cell body is externally connected to a corresponding nitrogen replacement pipe, and the nitrogen replacement pipe is connected to an external nitrogen source.

Advantages of the present invention:

1) The present invention replaces the product collection end from the electrolytic cell body to the refrigeration heat exchanger. On the basis of not affecting the normal operation of the refrigeration heat exchanger, an isolation area is formed at the bottom of the vertical heat exchange tank of the refrigeration heat exchanger through the setting of a multifunctional isolation mechanism. In the process of circulating refrigeration of the material in the vertical heat exchange tank, the product with a density greater than the electrolytic mother liquid will gradually be stored on the bottom side of the movable isolation part through the liquid permeable hole. When the height of the product stored at the bottom of the vertical heat exchange tank rises to the position of the plugging part, the plugging part begins to float until the height of the product stored at the bottom of the vertical heat exchange tank rises to the height of the top of the plugging part. The buoyancy of the plugging part is the largest. When the force acting on the pressure sensor under the action of its maximum buoyancy reaches the set value, it can be detected and judged that the storage amount of the high-density product stored at the bottom of the vertical heat exchange tank reaches the top height of the plugging part. At this time, the piston rod of the control driving hydraulic cylinder is retracted to drive the movable isolation part to squeeze and output the product stored on its bottom side from the product discharge pipe. During the product output process, the electrolysis process proceeds normally, so that the product can be output effectively and conveniently without affecting the electrolysis process, and the amount of entrainment of the electrolytic mother liquor during product output can be significantly reduced.

2) The middle part of the movable isolator of the present invention is connected downwardly with a retractable bellows, the bottom side of the retractable bellows is sleeved in the limiting tube, and the bottom end thereof is sealed and connected to the bottom of the heat exchange jacket. With the intervention of the retractable bellows and the limiting tube, the external installation of the isolator driving mechanism is realized, thereby preventing the material leakage caused by the driving of the movable isolator, thereby ensuring the practical effect of the present invention.

3) The heat exchange medium circulation mechanism of the present invention comprises a heat exchange jacket fixed to the outer side of the vertical heat exchange tank on the lower side of the lower partition in a sandwich state. During the refrigeration heat exchange process, the refrigerant is circulated through the heat exchange jacket in advance to cool the product material stored on the bottom side of the vertical heat exchange tank, so that the product material stored on the bottom side of the vertical heat exchange tank is always in a stable liquid state, thereby further ensuring the practical effect of the present invention.

4) The movable isolating member of the present invention is evenly filled with a plurality of corresponding vibration-reducing damping particles. Under the effect of friction energy dissipation between the vibration-reducing damping particles, a vibration-reducing isolation layer is effectively formed to reduce the fluctuation effect of the circulating liquid inlet process on the product stored at the bottom side of the vertical heat exchange tank, thereby reducing the probability of the circulating electrolyte mother liquid mixing into the product stored at the bottom side of the vertical heat exchange tank, so as to further reduce the entrainment of the electrolyte mother liquid when the product is output.

5) A corresponding siphon tee is connected to the product discharge pipe on the outside of the one-way valve of the present invention, and the siphon section of the siphon tee is connected to the bottom gap between the telescopic bellows and the limit tube. When the movable isolating member moves downward to squeeze and discharge the product stored on its bottom side from the product discharge pipe, the siphon tee forms a siphon on the gap between the telescopic bellows and the limit tube to pump and discharge the product between the telescopic bellows and the limit tube to the product discharge pipe, thereby forming a pressure relief on the gap between the telescopic bellows and the limit tube to prevent the telescopic bellows from being over-pressurized and causing obvious deformation, thereby further ensuring the practical effect of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG1 is a schematic structural diagram of the present invention.

FIG. 2 is a schematic diagram of the structure of a refrigeration heat exchanger.

FIG. 3 is a schematic structural diagram of a movable isolating member.

In the accompanying drawings: electrolytic cell body 1, mother liquor inlet pipe 2, vertical heat exchange tank 301, upper partition 302, lower partition 303, heat exchange circulation pipe 304, circulation feed pipe 4, circulation return pipe 5, one-way valve 6, product discharge pipe 7, heat exchange jacket 801, conducting pipe 802, refrigerant inlet pipe 803, refrigerant discharge pipe 804, movable isolation part 901, retractable bellows 902, limit pipe 903, blocking part 904, liquid permeable hole 10, driving hydraulic cylinder 11, pressure sensor 12, damping particles for vibration reduction 13, siphon tee 14, intermediate tank 15, exhaust gas discharge pipe 16, nitrogen replacement pipe 17.

DETAILED DESCRIPTION

In order to facilitate understanding by those skilled in the art, the structure of the present invention is further described in detail with reference to the embodiments and the accompanying drawings:

Referring to Figures 1-3, a perfluorotripropylamine electrolytic cell capable of detecting liquid density comprises:

An electrolytic cell body 1, a mother liquid inlet pipe 2 is provided outwardly on one side of the electrolytic cell body 1, and the electrolytic cell body 1 is an existing electrolytic cell device, which is an existing device and its specific structure is not described here;

A refrigeration heat exchanger, comprising a vertical heat exchange tank 301, wherein upper and lower sides of the vertical heat exchange tank 301 are respectively fixedly connected with corresponding upper partitions 302 and lower partitions 303, and a plurality of corresponding heat exchange circulation pipes 304 are connected through the upper partitions 302 and the lower partitions 303, wherein the vertical heat exchange tank 301 on the bottom side of the lower partition 303 is connected to the bottom of the electrolytic cell body 1 through a corresponding circulation feed pipe 4 pump, and the vertical heat exchange tank 301 on the upper side of the upper partition 302 is connected to the upper part of the electrolytic cell body 1 through a corresponding circulation return pipe 5, and the bottom end of the vertical heat exchange tank 301 is connected to the corresponding product discharge pipe 7 through a corresponding one-way valve 6;

The heat exchange medium circulation mechanism comprises a heat exchange jacket 801 fixedly connected to the outer side of the vertical heat exchange tank 301 on the lower side of the lower partition 303 in a sandwich state, a conducting pipe 802 connected to the vertical heat exchange tank 301 on the upper side of the lower partition 303 is provided on the upper part of the heat exchange jacket 801, a refrigerant inlet pipe 803 is connected to the bottom side of the heat exchange jacket 801, and a refrigerant outlet pipe 804 is connected to the vertical heat exchange tank 301 on the lower side of the upper partition 302;

The multifunctional isolation mechanism comprises a movable isolation member 901 disposed in the vertical heat exchange tank 301 below the circulating feed pipe 4, the middle of the movable isolation member 901 is downwardly connected with a retractable bellows 902, a corresponding limit tube 903 is installed between the vertical heat exchange tank 301 and the bottom of the heat exchange jacket 801, the bottom side of the retractable bellows 902 is sleeved in the limit tube 903, and the bottom end of the retractable bellows 902 is sealed and connected to the heat exchange jacket 801. The bottom of the sleeve 801; the movable isolating member 901 is provided with a plurality of corresponding mounting holes in an annular array, and a plurality of corresponding liquid permeable holes 10 are respectively provided around the mounting holes, and a blocking member 904 with an I-shaped cross section can be installed at the mounting holes in a lifting manner, and the density of the blocking member 904 is less than the density of the product and greater than the density of the mother liquid, and the bottom of the blocking member 904 can block the liquid permeable hole 10, and the top of the blocking member 904 does not block the liquid permeable hole 10;

The isolation member driving mechanism includes a driving hydraulic cylinder 11 arranged on the bottom side of the heat exchange jacket 801, the piston rod end of the driving hydraulic cylinder 11 is sleeved in the retractable bellows 902 and connected to the bottom side of the movable isolation member 901, and at least one corresponding pressure sensor 12 is provided on the movable isolation member 901, and one of the sealing members 904 floats up to form abutment and compression on the pressure sensor 12. When the height of the product stored at the bottom of the vertical heat exchange tank 301 rises to the height of the top of the sealing member 904, the sealing member 904 exerts a force on the pressure sensor 12 under the action of its maximum buoyancy to reach a set value, and the piston rod of the driving hydraulic cylinder 11 retracts to drive the movable isolation member 901 to squeeze and output the product stored on its bottom side from the product discharge pipe 7.

The present invention replaces the product collection end from the electrolytic cell body 1 with the refrigeration heat exchanger. On the basis of not affecting the normal operation of the refrigeration heat exchanger, the multifunctional isolation mechanism is set to form an isolation area at the bottom of the vertical heat exchange tank 301 of the refrigeration heat exchanger. During the process of circulating refrigeration of the material in the vertical heat exchange tank 301, the product with a density greater than the electrolytic mother liquid will gradually pass through the liquid permeable hole 10 to form storage on the bottom side of the movable isolation member 901. When the height of the product stored at the bottom of the vertical heat exchange tank 301 rises to the position of the blocking member 904, the blocking member 904 It starts to float until the height of the product stored at the bottom of the vertical heat exchange tank 301 rises to the height of the top of the plugging member 904. The buoyancy of the plugging member 904 is the largest. When the force acting on the pressure sensor 12 under the action of its maximum buoyancy reaches the set value, it can be detected and judged that the storage volume of the high-density product stored at the bottom of the vertical heat exchange tank 301 reaches the top height of the plugging member 904. At this time, the piston rod of the control driving hydraulic cylinder 11 is retracted to drive the movable isolation member 901 to squeeze and output the product stored at its bottom side from the product discharge pipe 7. During the product output process, the electrolysis process is carried out normally, so that the product can be effectively and conveniently output without affecting the electrolysis process, and the entrainment of the electrolytic mother liquor during the product output can be significantly reduced.

The present invention realizes the external installation of the isolator drive mechanism with the intervention of the telescopic bellows 902 and the limit tube 903, thereby preventing the material leakage caused by the driving of the movable isolator 901, so as to ensure the practical effect of the present invention. In the refrigeration heat exchange process of the present invention, the refrigerant is circulated through the heat exchange jacket 801 in advance to cool the product material stored at the bottom side of the vertical heat exchange tank 301, so that the product material stored at the bottom side of the vertical heat exchange tank 301 is always in a stable liquid state, thereby ensuring the practical effect of the present invention.

The movable isolating member 901 is evenly filled with a plurality of corresponding vibration damping particles 13. In this embodiment, the vibration damping particles 13 are iron spherical particles. Under the friction energy dissipation between the vibration damping particles 13, a vibration damping isolation layer is effectively formed to reduce the fluctuation effect of the circulating liquid inlet process on the product stored at the bottom of the vertical heat exchange tank 301, thereby reducing the probability of the circulating electrolytic mother liquid being mixed into the product stored at the bottom of the vertical heat exchange tank 301, so as to further reduce the entrainment of the electrolytic mother liquid when the product is output.

A corresponding siphon tee 14 is connected to the product discharge pipe 7 outside the one-way valve 6, and the siphon section of the siphon tee 14 is connected to the bottom interval between the telescopic bellows 902 and the limiting pipe 903. When the movable isolating member 901 moves downward to squeeze and output the product stored at the bottom side thereof from the product discharge pipe 7, the siphon tee 14 forms a siphon on the interval between the telescopic bellows 902 and the limiting pipe 903, so as to pump and discharge the product between the telescopic bellows 902 and the limiting pipe 903 to the product discharge pipe 7, thereby forming a pressure relief on the interval between the telescopic bellows 902 and the limiting pipe 903, so as to prevent the telescopic bellows 902 from being over-pressurized and causing obvious deformation, thereby further ensuring the practical effect of the present invention.

The signal line of the pressure sensor 12 passes through the retractable bellows 902 and is connected to an external electrical controller.

The product discharge pipe 7 is connected to the corresponding intermediate tank 15. The intermediate tank 15 is pumped to the feed end of the corresponding distillation equipment.

The upper right side of the electrolytic cell body 1 is connected to an exhaust gas exhaust pipe 16. The left side of the electrolytic cell body 1 is connected to a corresponding nitrogen replacement pipe 17, which is connected to an external nitrogen source. Before the electrolysis process begins, nitrogen is introduced into the electrolytic cell body 1 through the nitrogen replacement pipe 17 to perform nitrogen replacement.

The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims (8)

1. A perfluorotripropylamine electrolytic cell capable of detecting liquid density, characterized in that it comprises: An electrolytic cell body (1), wherein a mother liquid inlet pipe (2) is disposed outwardly on one side of the electrolytic cell body (1); A refrigeration heat exchanger, comprising a vertical heat exchange tank (301), wherein the upper and lower sides of the vertical heat exchange tank (301) are respectively fixedly connected with corresponding upper baffles (302) and lower baffles (303), and a plurality of corresponding heat exchange circulation pipes (304) are connected through the upper baffles (302) and the lower baffles (303); the vertical heat exchange tank (301) on the bottom side of the lower baffle (303) is pumped to the bottom of the electrolytic cell body (1) through a corresponding circulation feed pipe (4), and the vertical heat exchange tank (301) on the upper side of the upper baffle (302) is connected to the upper part of the electrolytic cell body (1) through a corresponding circulation return pipe (5); and the bottom end of the vertical heat exchange tank (301) is externally connected to a corresponding product discharge pipe (7) through a corresponding one-way valve (6); The heat exchange medium circulation mechanism comprises a heat exchange jacket (801) fixedly connected to the outer side of the vertical heat exchange tank (301) on the lower side of the lower partition (303) in a sandwich state, a conducting pipe (802) connected to the vertical heat exchange tank (301) on the upper side of the lower partition (303) is provided on the upper part of the heat exchange jacket (801), a refrigerant inlet pipe (803) is connected to the bottom side of the heat exchange jacket (801), and a refrigerant outlet pipe (804) is connected to the vertical heat exchange tank (301) on the lower side of the upper partition (302); The multifunctional isolation mechanism comprises a movable isolation member (901) arranged in a vertical heat exchange tank (301) below the circulating feed pipe (4); a retractable bellows (902) is connected downwardly to the middle of the movable isolation member (901); a corresponding limiting pipe (903) is installed between the bottom of the vertical heat exchange tank (301) and the heat exchange jacket (801); the bottom side of the retractable bellows (902) is sleeved in the limiting pipe (903); and the bottom end of the retractable bellows (902) is sealed and connected to the vertical heat exchange tank (301). The bottom of the heat jacket (801); the movable isolating member (901) is provided with a plurality of corresponding mounting holes in an annular array, and a plurality of corresponding liquid permeable holes (10) are respectively provided around the mounting holes; and sealing members (904) with an I-shaped cross section are respectively installed at the mounting holes in a manner that they can be lifted and lowered, and the density of the sealing member (904) is less than the density of the product and greater than the density of the mother liquid, and the bottom of the sealing member (904) can form a blockage for the liquid permeable holes (10), and the top of the sealing member (904) does not form a blockage for the liquid permeable holes (10); The isolating member driving mechanism comprises a driving hydraulic cylinder (11) arranged at the bottom side of the heat exchange jacket (801), the piston rod end of the driving hydraulic cylinder (11) being sleeved in the retractable bellows (902) and connected to the bottom side of the movable isolating member (901), and at least one corresponding pressure sensor (12) being arranged on the movable isolating member (901), wherein one of the sealing members (904) floats up to a position to form abutment and compression against the pressure sensor (12), and when the height of the product stored at the bottom of the vertical heat exchange tank (301) rises to the height where the top of the sealing member (904) is located, the force exerted by the sealing member (904) on the pressure sensor (12) under the action of its maximum buoyancy reaches a set value, and the piston rod of the driving hydraulic cylinder (11) retracts to drive the movable isolating member (901) to squeeze and output the product stored at the bottom side thereof from the product discharge pipe (7). 2. A perfluorotripropylamine electrolytic cell capable of detecting liquid density according to claim 1, characterized in that a plurality of corresponding vibration-reducing damping particles (13) are evenly filled and installed in the movable isolation member (901). 3. A perfluorotripropylamine electrolytic cell capable of detecting liquid density according to claim 1, characterized in that a corresponding siphon tee (14) is connected to the product discharge pipe (7) outside the one-way valve (6), and the siphon section of the siphon tee (14) is connected to the bottom gap between the retractable bellows (902) and the limiting tube (903). 4. A perfluorotripropylamine electrolytic cell capable of detecting liquid density according to claim 1, characterized in that a signal line of the pressure sensor (12) passes through the retractable bellows (902) and is connected to an external electrical controller. 5. A perfluorotripropylamine electrolytic cell capable of detecting liquid density according to claim 1, characterized in that the product discharge pipe (7) is connected to a corresponding intermediate tank (15). 6. A perfluorotripropylamine electrolytic cell capable of detecting liquid density according to claim 5, characterized in that the intermediate tank (15) is pumped to the feed end of the corresponding distillation equipment. 7. A perfluorotripropylamine electrolytic cell capable of detecting liquid density according to claim 1, characterized in that an exhaust gas exhaust pipe (16) is externally connected to the upper right side of the electrolytic cell body (1). 8. A perfluorotripropylamine electrolytic cell capable of detecting liquid density according to claim 7, characterized in that the left side of the electrolytic cell body (1) is externally connected to a corresponding nitrogen displacement tube (17), and the nitrogen displacement tube (17) is connected to an external nitrogen source.