CN211366951U - Synthesis reactor of iodine pentafluoride - Google Patents

Synthesis reactor of iodine pentafluoride Download PDF

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Publication number
CN211366951U
CN211366951U CN201922389646.4U CN201922389646U CN211366951U CN 211366951 U CN211366951 U CN 211366951U CN 201922389646 U CN201922389646 U CN 201922389646U CN 211366951 U CN211366951 U CN 211366951U
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iodine
inlet
reactor
outlet
fluorine
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韩保国
李博文
崔武孝
阎晓冬
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Luoyang Sunland Chem Sci&tech Co ltd
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Luoyang Sunland Chem Sci&tech Co ltd
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Abstract

A synthesis reactor of iodine pentafluoride is provided with a fluorine inlet, a feed inlet, a cooling liquid outlet, an air outlet, a cooling liquid inlet and a liquid inlet and outlet; a liquid flow pipe communicated with the liquid inlet and the liquid outlet, a fluorine flow pipe with an inlet communicated with the fluorine inlet and an outlet extending to the bottom of the iodine pentafluoride solution, a cold coil pipe positioned above the liquid level of the solution and a baffle plate are arranged in the liquid flow pipe; a constant temperature cooling device is arranged on the outer side of the shell; the cold coil is communicated with the cooling liquid inlet and the cooling liquid outlet. The utility model has the advantages that the fluorine gas bubbling pipe is arranged to ensure that the fluorine gas bubbles and the iodine dissolved in the iodine pentafluoride solution and the iodine not dissolved at the bottom are directly reacted, thereby improving the reaction efficiency; the iodine sublimated in the reaction process can be condensed and attached to the cooling coil and the baffle plate on the liquid surface, and the incompletely reacted fluorine gas can be reacted with the iodine attached to the cooling coil or the baffle plate again to generate iodine pentafluoride in the process of flowing to the air outlet, so that the problem that the iodine simple substance blocks the distribution pipe is effectively solved, and the utilization rate of the fluorine gas is also improved.

Description

Synthesis reactor of iodine pentafluoride
Technical Field
The utility model relates to a novel reactor for synthesizing iodine pentafluoride (IF5) by using reaction of iodine and fluorine gas.
Background
The most main current uses of iodine pentafluoride are raw materials in the production of fluorine-containing surfactants and oil-proof and water-proof textile treating agents, and raw materials of perfluoroiodoalkane and the like for synthesizing the fluorine-containing surfactants and fluorine-containing textile finishing agents.
The prior common method for synthesizing iodine pentafluoride mainly comprises two forms of direct reaction of fluorine gas introduced into iodine or reaction of fluorine gas introduced into iodine pentafluoride solution dissolved with iodine.
When the fluorine gas directly reacts with the iodine to generate the iodine pentafluoride, the reaction heat value is large, so that the local temperature of the position of a reaction point is obviously increased, on one hand, the requirement on the quality of a reactor is high due to high temperature, and on the other hand, the iodine can be rapidly sublimated at a piping to desublimate and block the pipeline due to the high temperature.
The method solves the problem of reaction heat aggregation by introducing fluorine gas after iodine is dissolved in iodine pentafluoride solution, but the reaction efficiency is limited due to low solubility of iodine in iodine pentafluoride, and meanwhile, iodine also has sublimation phenomenon to block pipelines.
Disclosure of Invention
For overcoming the problem that the iodine that is difficult to handle among the prior art sublimes and blocks up the pipeline, the utility model aims to provide a can make full use of fluorine gas and pollute few iodine pentafluoride synthesis reactor.
The utility model aims at adopting the following technical scheme to realize. According to the synthesis reactor of iodine pentafluoride provided by the utility model, the reactor is provided with a fluorine inlet, a charging opening, a cooling liquid outlet, a gas outlet, a cooling liquid inlet, a liquid inlet and a liquid outlet; the reactor is internally provided with a liquid flow pipe which is communicated with the liquid inlet and the liquid outlet so as to suck iodine pentafluoride solution into the reactor before the synthesis reaction starts and extrude the iodine pentafluoride solution out of the reactor after the synthesis reaction finishes, a fluorine flow pipe of which the inlet is communicated with the fluorine inlet and the outlet extends to the bottom of the iodine pentafluoride solution so as to ensure that fluorine introduced from the fluorine inlet bubbles and directly reacts with iodine dissolved in the iodine pentafluoride solution and iodine not dissolved at the bottom, and a cooling coil and a baffle plate which are positioned above the liquid level of the iodine pentafluoride solution and are used for enabling the iodine sublimated in the reaction process to be condensed and adhered and then to react with the incompletely reacted fluorine again; the cold coil is communicated with the cooling liquid inlet and the cooling liquid outlet; the reactor is provided with a pressure sensor for detecting the internal pressure of the reactor and a first temperature sensor for detecting the reaction temperature, and a pipeline of the cooling liquid outlet is provided with a second temperature sensor for detecting the temperature of the cooling liquid flowing out of the cooling liquid outlet; the outer side of the reactor is provided with a constant temperature cooling device which is used for taking away the heat generated by the direct reaction of the fluorine gas and the undissolved iodine so as to control the reaction temperature.
Furthermore, a fluorine inlet, a charging opening, a cooling liquid outlet, an air outlet and a cooling liquid inlet are all arranged at the top of the reactor.
Furthermore, the constant temperature cooling device comprises a constant temperature jacket arranged outside the reactor, a constant temperature water inlet and a constant temperature water outlet which are communicated with the constant temperature jacket.
Further, the constant temperature water inlet is positioned at the lower side of the constant temperature water outlet.
The utility model provides a synthetic reactor of iodine pentafluoride has following advantage:
1. the fluorine gas introduced from the fluorine inlet is bubbled through the fluorine gas flow pipe to directly react with the iodine dissolved in the iodine pentafluoride solution and the iodine not dissolved at the bottom, so that the reaction efficiency is improved;
2. the iodine sublimated in the reaction process can be condensed and attached to the cooling coil and the baffle plate on the liquid surface, and the incompletely reacted fluorine gas can be reacted with the iodine attached to the cooling coil or the baffle plate again to generate iodine pentafluoride in the process of flowing to the air outlet, so that the problem that the iodine simple substance blocks the piping is effectively solved, and the utilization rate of the fluorine gas is also improved;
3. in the reaction process, the tail gas discharged from the gas outlet is tested by adopting moist starch potassium iodide test paper, and the test paper does not change color. The tail gas is discharged after being adsorbed by the adsorption tower, and no pollution is caused.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented according to the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more obvious and understandable, the following preferred embodiments are described in detail with reference to the accompanying drawings.
Drawings
Fig. 1 is a schematic structural diagram of a synthesis reactor for iodine pentafluoride according to the present invention.
[ description of main element symbols ]
1-reactor 2-fluorine inlet 3-charging port 4-cooling liquid outlet 5-gas outlet
6-cooling liquid inlet 7-liquid inlet and outlet 8-constant temperature water inlet 9-constant temperature water outlet 10-constant temperature jacket
11-baffle plate 12-cold coil 13-pressure sensor 14-first temperature sensor 15-second temperature sensor
Detailed Description
The technical solution of the present invention will be further explained with reference to the accompanying drawings and preferred embodiments.
Referring to fig. 1, the present invention relates to an iodine pentafluoride synthesis reactor, which has a fluorine inlet 2, a charging opening 3, a coolant outlet 4, a gas outlet 5, a coolant inlet 6, and a liquid inlet and outlet 7 for allowing iodine pentafluoride solution to enter or leave the reactor, wherein the fluorine inlet 2, the charging opening 3, the coolant outlet 4, the gas outlet 5, and the coolant inlet 6 are all installed at the top of the reactor 1, and of course, in other embodiments, the present invention can be adjusted according to the production requirement. A fluorine flow pipe is arranged in the reactor 1, the inlet of the fluorine flow pipe is communicated with the fluorine inlet 2, the outlet of the fluorine flow pipe extends to the bottom of the iodine pentafluoride solution contained in the reactor, iodine elementary substance can be dissolved in the iodine pentafluoride solution at normal temperature and normal pressure, therefore, excessive iodine elementary substance is added into the reactor through the feed port 3, more iodine can be dissolved in the iodine pentafluoride solution to form a reddish brown solution, part of undissolved iodine can be deposited at the bottom of the iodine pentafluoride solution, and at the moment, the outlet of the fluorine flow pipe is inserted to the bottom of the solution, so that bubbling entering the reactor through the fluorine inlet directly reacts with the iodine dissolved in the iodine pentafluoride solution and the undissolved iodine at the bottom of the solution, and the reaction efficiency is improved; the reactor 1 is also internally provided with a liquid flow pipe which is communicated with the liquid inlet and outlet 7 so as to allow the iodine pentafluoride solution to enter the reactor before the synthesis reaction starts and allow the iodine pentafluoride solution to leave the reactor after the synthesis reaction is finished; a plurality of baffle plates 11 which are distributed in parallel from top to bottom and are positioned above the liquid level of the iodine pentafluoride solution are also arranged in the reactor 1, and the baffle plates are arranged at the top of the reactor through support rods; the reactor 1 is also internally provided with a cold coil 12 positioned above the liquid level of the iodine pentafluoride solution, and the cold coil 12 is arranged at the top of the reactor and is respectively communicated with a cooling liquid inlet 6 and a cooling liquid outlet 4. The reactor 1 is provided with a pressure sensor 13 for detecting the internal pressure of the reactor and a first temperature sensor 14 for detecting the reaction temperature, and the pipe of the cooling liquid outlet 4 is provided with a second temperature sensor 15 for detecting the temperature of the cooling liquid flowing out from the cooling liquid outlet. The outer side of the reactor 1 is annularly provided with a constant temperature cooling device, the constant temperature cooling device in the embodiment comprises a constant temperature jacket 10 arranged on the outer side of the reactor, a constant temperature water inlet 8 and a constant temperature water outlet 9 which are communicated with the constant temperature jacket, the constant temperature water inlet is positioned below the constant temperature water outlet, and heat generated by direct reaction of fluorine gas and iodine is taken away through the circulating flow of constant temperature water during synthesis reaction so as to control the reaction temperature.
The utility model relates to a synthetic reactor of iodine pentafluoride's working process as follows: firstly purifying a reactor → then sealing the reactor and performing vacuum-pumping replacement on the reactor to keep negative pressure → then sucking the iodine pentafluoride solution into the reactor 1 through a liquid inlet and outlet 7, adding excessive iodine simple substance (the adding weight is 10-30% of the total weight of the iodine pentafluoride solution) into the reactor 1 through a feeding port 3 → then introducing cooling liquid into a cold coil 12 through a cooling liquid inlet 6, introducing constant-temperature water into a constant-temperature jacket 10 through a constant-temperature water inlet 9 → then introducing fluorine gas into the reactor 1 through a fluorine inlet 2, so that the fluorine gas is bubbled in the iodine pentafluoride solution to react with iodine. In the reaction process, the iodine is rapidly sublimated by the heat generated by the reaction, the sublimated iodine almost completely condenses and adheres to the low-temperature cold coil 12 and the baffle plate 11 after encountering the low-temperature cold coil and the baffle plate on the liquid surface, and the incompletely reacted fluorine gas can react with iodine simple substances adhered to the cold coil 12 and the baffle plate 11 again to generate iodine pentafluoride in the process of flowing to the air outlet 5 and then flows into the iodine pentafluoride solution below along the walls of the cold coil and the baffle plate, so that the problem that the iodine simple substances block the piping is effectively solved, the utilization rate of the fluorine gas is also improved, and the conversion rate of the product is improved; in the reaction process, moist starch potassium iodide test paper is used for testing the tail gas discharged from the gas outlet 5, the test paper does not change color, the tail gas basically does not contain fluorine gas, the tail gas is absorbed by an absorption tower and then is discharged, so that the pollution of the tail gas is reduced → the reactor 1 is filled with nitrogen for pressurization after the reaction is finished, and the iodine pentafluoride solution is extruded through the liquid inlet and outlet 7. Through measurement, the synthesized iodine pentafluoride product is colorless and transparent, and the purity of the iodine pentafluoride product is as high as 99%. Opening the reactor additionally found: the pipeline at the air outlet is basically free from the attachment of solid iodine, and a small amount of iodine pentafluoride liquid residue is left on the cold coil.
As described above, the present invention is only a preferred embodiment of the present invention, and any person skilled in the art can easily modify, change or modify the above embodiments according to the technical essence of the present invention without departing from the scope of the present invention.

Claims (4)

1. A synthesis reactor of iodine pentafluoride is characterized in that the reactor is provided with a fluorine inlet, a feed inlet, a cooling liquid outlet, an air outlet, a cooling liquid inlet and a liquid inlet and outlet; the reactor is internally provided with a liquid flow pipe which is communicated with the liquid inlet and the liquid outlet so as to suck iodine pentafluoride solution into the reactor before the synthesis reaction starts and extrude the iodine pentafluoride solution out of the reactor after the synthesis reaction finishes, a fluorine flow pipe of which the inlet is communicated with the fluorine inlet and the outlet extends to the bottom of the iodine pentafluoride solution so as to ensure that fluorine introduced from the fluorine inlet bubbles and directly reacts with iodine dissolved in the iodine pentafluoride solution and iodine not dissolved at the bottom, and a cooling coil and a baffle plate which are positioned above the liquid level of the iodine pentafluoride solution and are used for enabling the iodine sublimated in the reaction process to be condensed and adhered and then to react with the incompletely reacted fluorine again; the cold coil is communicated with the cooling liquid inlet and the cooling liquid outlet; the reactor is provided with a pressure sensor for detecting the internal pressure of the reactor and a first temperature sensor for detecting the reaction temperature, and a pipeline of the cooling liquid outlet is provided with a second temperature sensor for detecting the temperature of the cooling liquid flowing out of the cooling liquid outlet; the outer side of the reactor is provided with a constant temperature cooling device which is used for taking away the heat generated by the direct reaction of the fluorine gas and the undissolved iodine so as to control the reaction temperature.
2. The reactor for synthesizing iodine pentafluoride according to claim 1, wherein the fluorine inlet, the feed inlet, the cooling liquid outlet, the gas outlet and the cooling liquid inlet are all arranged at the top of the reactor.
3. The reactor for synthesizing iodine pentafluoride according to claim 1, wherein the constant temperature cooling means comprises a constant temperature jacket installed outside the reactor, a constant temperature water inlet and a constant temperature water outlet communicated with the constant temperature jacket.
4. The reactor for synthesizing iodine pentafluoride according to claim 3, wherein the constant-temperature water inlet is located at a lower side of the constant-temperature water outlet.
CN201922389646.4U 2019-12-26 2019-12-26 Synthesis reactor of iodine pentafluoride Active CN211366951U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112537755A (en) * 2020-12-16 2021-03-23 中船重工(邯郸)派瑞特种气体有限公司 Preparation method and device of iodine pentafluoride
CN114950301A (en) * 2022-05-31 2022-08-30 中船(邯郸)派瑞特种气体股份有限公司 Iodine pentafluoride synthesizer

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112537755A (en) * 2020-12-16 2021-03-23 中船重工(邯郸)派瑞特种气体有限公司 Preparation method and device of iodine pentafluoride
CN114950301A (en) * 2022-05-31 2022-08-30 中船(邯郸)派瑞特种气体股份有限公司 Iodine pentafluoride synthesizer
CN114950301B (en) * 2022-05-31 2023-05-02 中船(邯郸)派瑞特种气体股份有限公司 Iodine pentafluoride synthesizer

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