CN216404257U - Device for removing small amount of fluorine-containing olefin in octafluorocyclobutane - Google Patents

Device for removing small amount of fluorine-containing olefin in octafluorocyclobutane Download PDF

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CN216404257U
CN216404257U CN202122007310.4U CN202122007310U CN216404257U CN 216404257 U CN216404257 U CN 216404257U CN 202122007310 U CN202122007310 U CN 202122007310U CN 216404257 U CN216404257 U CN 216404257U
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outlet
inlet
tower
communicated
adsorption column
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钱厚琴
胡经宇
徐�明
吴玉勋
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Taixing Meilan New Material Co ltd
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Taixing Meilan New Material Co ltd
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Abstract

The utility model discloses a device for removing a small amount of fluorine-containing olefin in octafluorocyclobutane, wherein an oxygen conveying pipe (7) extends into a reaction kettle (1), an outlet I (8) of the reaction kettle (1) is communicated with an inlet II (9) of a vaporizer (2) through a conveying pipe I (10), an outlet II (11) at the top of the vaporizer (2) is communicated with an inlet III (12) at the side of an alkaline tower (3) through a conveying pipe II (13), an outlet III (14) at the top of the alkaline tower (3) is communicated with an inlet IV (15) at the side of a water washing tower (4) through a conveying pipe III (16), an outlet IV (17) at the top of the water washing tower (4) is communicated with an inlet V (18) at the side of a rectifying tower (5) through an adsorption device, and an outlet V (20) is arranged at the side of a redistributor (19) at the tower body of the rectifying tower (5). The utility model can achieve the effect of purifying octafluorocyclobutane.

Description

Device for removing small amount of fluorine-containing olefin in octafluorocyclobutane
Technical Field
The utility model relates to a device for removing a small amount of fluorine-containing olefin in octafluorocyclobutane.
Background
Octafluorocyclobutane (abbreviated as C318 under the name Octafluorocyclobutane) has the formula CF2CF2CF2CF 2. The high-voltage insulating material has stable property, no toxicity, zero Ozone Depletion Potential (ODP), good insulating property and the like, and is widely applied to the technical fields of high-voltage insulation, cleaning and etching, plasma treatment and the like in recent years. The C318 used as the plasma etching agent requires extremely high purity, at least reaching 99.999 percent (mol) purity, the gas with the purity is generally called electronic grade gas, the defect rate of manufacturing high-density integrated circuits can be increased by very little impurity, the octafluorocyclobutane removes the fluorine-containing olefin impurity, the octafluorocyclobutane produced by thermal cracking tetrafluoroethylene is not suitable for recovering the octafluorocyclobutane obtained in the process of preparing tetrafluoroethylene by cracking difluorochloromethane, and at present, no device for removing a small amount of fluorine-containing olefin in the octafluorocyclobutane is available.
Disclosure of Invention
The utility model provides a device for removing a small amount of fluorine-containing olefin in octafluorocyclobutane, which oxidizes fluorine-containing olefin impurities into polyether acyl fluoride, and is washed by alkaline water for dehydration and rectification so as to achieve the effect of purifying the octafluorocyclobutane.
The utility model adopts the following technical scheme: a device for removing a small amount of fluorine-containing olefin in octafluorocyclobutane mainly comprises a reaction kettle, a vaporizer, an alkaline tower, a water washing tower, an adsorption device and a rectifying tower, wherein the top of the reaction kettle is provided with an inlet I, an oxygen conveying pipe extends into the reaction kettle through the inlet I, the bottom of the reaction kettle is provided with an outlet I, the bottom of the vaporizer is provided with an inlet II, the outlet I is communicated with the inlet II through a conveying pipe I, the top of the vaporizer is provided with an outlet II, the side surface of the alkaline tower is provided with an inlet III, the outlet II is communicated with the inlet III through a conveying pipe II, the top of the alkaline tower is provided with an outlet III, the side surface of the water washing tower is provided with an inlet IV, the outlet III is communicated with the inlet IV through a conveying pipe III, the top of the water washing tower is provided with an outlet IV, the outlet IV is communicated with a side surface inlet V of the rectifying tower through the adsorption device, and the bottom of the rectifying tower body is provided with a redistributor, the side of the redistributor is provided with an outlet V.
The reaction kettle is a photo-oxidation reaction kettle. The vaporizer is a pressure vaporizer or a floating vaporizer. The adsorption device comprises an adsorption column I, an adsorption column II, an adsorption column III and an adsorption column IV, an outlet IV is communicated with a feed inlet of the adsorption column I, the adsorption column I is sequentially connected with the adsorption column II, the adsorption column III and the adsorption column IV in series through adsorption tubes, and a discharge outlet of the adsorption column IV is communicated with an inlet V.
The rectifying tower is a filler rectifying tower. The rectification packing in the packing rectification tower is metal Dixon packing, metal pall ring packing or metal structured packing, and the height of the rectification packing is 5-30 m.
The utility model has the following beneficial effects: after the technical scheme is adopted, the utility model leads the fluorine-containing olefin impurities to be oxidized into polyether acyl fluoride, and the octafluorocyclobutane is purified by introducing the alkaline washing water for dehydration and rectification. The equipment of the utility model can improve the removal efficiency, has good removal effect and reduces the loss.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Detailed Description
In figure 1, the utility model provides a device for removing a small amount of fluorine-containing olefin from octafluorocyclobutane, which mainly comprises a reaction kettle 1, a vaporizer 2, an alkaline tower 3, a water scrubber 4, an adsorption device and a rectifying tower 5, wherein the reaction kettle 1 is set as a photooxidation reaction kettle, the vaporizer 2 is set as a pressure vaporizer or a floating vaporizer, the top of the reaction kettle 1 is provided with an inlet I6, an oxygen conveying pipe 7 extends into the reaction kettle 1 through the inlet I6, the bottom of the reaction kettle 1 is provided with an outlet I8, the bottom of the vaporizer 2 is provided with an inlet II 9, the outlet I8 is communicated with the inlet II 9 through a conveying pipe I10, the top of the vaporizer 2 is provided with an outlet II 11, the side of the alkaline tower 3 is provided with an inlet III 12, the outlet II 11 is communicated with the inlet III 12 through a conveying pipe II 13, the top of the alkaline tower 3 is provided with an outlet III 14, an inlet IV 15 is arranged on the side surface of the water washing tower 4, the outlet III 14 is communicated with the inlet IV 15 through a conveying pipe III 16, an outlet IV 17 is arranged at the top of the water washing tower 4, the outlet IV 17 is communicated with an inlet V18 on the side surface of the rectifying tower 5 through an adsorption device, the adsorption device comprises an adsorption column I21, an adsorption column II 22, an adsorption column III 23 and an adsorption column IV 24, the outlet IV 17 is communicated with a feed inlet of the adsorption column I21, the adsorption column I21 is sequentially connected with the adsorption column II 22, the adsorption column III 23 and the adsorption column IV 24 in series through an adsorption pipe 25, a discharge port of the adsorption column IV 24 is communicated with the inlet V18, a redistributor 19 is arranged at the bottom of the rectifying tower 5, an outlet V20 is arranged on the side surface of the redistributor 19, the rectifying tower 5 is provided with a filler rectifying tower, and the rectifying filler in the rectifying tower is a metal Dieck pine filler, The height of the rectification packing is 5-30 m.
The use method of the utility model comprises the following steps: firstly, introducing a high-purity oxygen conveying pipe 7 into a photo-oxidation reaction kettle of octafluorocyclobutane with a small amount of fluorine-containing olefin, and converting impurities of the fluorine-containing olefin into polyether acyl fluoride after an ultraviolet light irradiation reaction at a stirring speed of a certain temperature and pressure, wherein the octafluorocyclobutane does not participate in the reaction due to stable properties;
and step two, after the octafluorocyclobutane solution containing the polyether acyl fluoride is vaporized by a vaporizer 2, passes through alkaline washing of an alkaline washing tower 3, water washing of a water washing tower 4 and adsorption and dehydration by an adsorption device, an adsorbent for adsorption is one or more of silica gel, a molecular sieve, solid caustic soda and concentrated sulfuric acid, and is rectified and purified by a filler rectifying tower to obtain the purified octafluorocyclobutane solution, wherein the fluorine-containing olefin impurity in the octafluorocyclobutane solution is less than 10 ppm.

Claims (6)

1. A device for removing a small amount of fluorine-containing olefin in octafluorocyclobutane is characterized by mainly comprising a reaction kettle (1), a vaporizer (2), an alkaline washing tower (3), a water washing tower (4), an adsorption device and a rectifying tower (5), wherein the top of the reaction kettle (1) is provided with an inlet I (6), an oxygen conveying pipe (7) extends into the reaction kettle (1) through the inlet I (6), the bottom of the reaction kettle (1) is provided with an outlet I (8), the bottom of the vaporizer (2) is provided with an inlet II (9), the outlet I (8) is communicated with the inlet II (9) through a conveying pipe I (10), the top of the vaporizer (2) is provided with an outlet II (11), the side surface of the alkaline washing tower (3) is provided with an inlet III (12), the outlet II (11) is communicated with the inlet III (12) through a conveying pipe II (13), the top of the alkaline washing tower (3) is provided with an outlet (14), the side of the water washing tower (4) is provided with an inlet IV (15), the outlet III (14) and the inlet IV (15) are communicated through a conveying pipe III (16), the top of the water washing tower (4) is provided with an outlet IV (17), the outlet IV (17) is communicated with an inlet V (18) on the side of the tower body of the rectifying tower (5) through an adsorption device, the bottom of the tower body of the rectifying tower (5) is provided with a redistributor (19), and the side of the redistributor (19) is provided with an outlet V (20).
2. The apparatus for removing a small amount of fluorine-containing olefin in octafluorocyclobutane according to claim 1, wherein the reaction vessel (1) is a photo-oxidation reaction vessel.
3. The apparatus for removing a small amount of fluoroolefin from octafluorocyclobutane according to claim 1, wherein said vaporizer (2) is a pressure type vaporizer or a floating type vaporizer.
4. The device for removing a small amount of fluorine-containing olefin in octafluorocyclobutane according to claim 1, wherein the adsorption device comprises an adsorption column I (21), an adsorption column II (22), an adsorption column III (23) and an adsorption column IV (24), the outlet IV (17) is communicated with the feed inlet of the adsorption column I (21), the adsorption column I (21) is sequentially connected in series with the adsorption column II (22), the adsorption column III (23) and the adsorption column IV (24) through an adsorption tube (25), and the discharge outlet of the adsorption column IV (24) is communicated with the inlet V (18).
5. The apparatus for removing a small amount of fluorine-containing olefin in octafluorocyclobutane according to claim 1, wherein said rectifying column (5) is a packed rectifying column.
6. The device for removing a small amount of fluorine-containing olefin in octafluorocyclobutane according to claim 5, wherein the rectification packing in the packing rectification column is metal Dirichon packing, metal pall ring packing or metal structured packing, and the height of the rectification packing is 5-30 m.
CN202122007310.4U 2021-08-25 2021-08-25 Device for removing small amount of fluorine-containing olefin in octafluorocyclobutane Active CN216404257U (en)

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Application Number Priority Date Filing Date Title
CN202122007310.4U CN216404257U (en) 2021-08-25 2021-08-25 Device for removing small amount of fluorine-containing olefin in octafluorocyclobutane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202122007310.4U CN216404257U (en) 2021-08-25 2021-08-25 Device for removing small amount of fluorine-containing olefin in octafluorocyclobutane

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CN216404257U true CN216404257U (en) 2022-04-29

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