CN217067708U

CN217067708U - Fluorine-containing byproduct recovery system

Info

Publication number: CN217067708U
Application number: CN202220522544.4U
Authority: CN
Inventors: 刘桢; 万仁军; 王顺好; 张宗林; 杨建全
Original assignee: Sichuan Xiaifu Technology Co ltd
Current assignee: Sichuan Xiaifu Technology Co ltd
Priority date: 2022-03-10
Filing date: 2022-03-10
Publication date: 2022-07-29
Anticipated expiration: 2032-03-10

Abstract

The utility model provides a fluorine-containing byproduct recovery system, the purpose is the separation of other mixtures, recovery processing's problem in solving among the prior art fluorine-containing fine chemical products production process. Provided is a fluorine-containing byproduct recovery system including: a mixture washing column; the mixture washing water settling tank is communicated with the mixture washing tower; the sediment rectifying tower is communicated with the mixture washing water settling tank; the first refrigerant heat exchanger is communicated with the sediment rectifying tower; the rectification byproduct storage tank is communicated with the first refrigerant heat exchanger, and the kettle bottom product collection tank is communicated with the sediment rectification tower; the organic auxiliary agent rectifying tower is communicated with the mixture washing water settling tank; the second refrigerant heat exchanger is communicated with the organic auxiliary agent rectifying tower; the organic auxiliary agent recovery storage tank is communicated with the second refrigerant heat exchanger. The utility model discloses a to the recovery that organic auxiliary agent and fluorine-containing by-product were realized to by-product mixture collection, alkali lye washing water washing, washing mixture sedimentation separation, washing liquid rectification separation, deposit distillation separation and condensation.

Description

Fluorine-containing byproduct recovery system

Technical Field

The utility model belongs to the technical field of fluorine recovery technique and specifically relates to a fluorine-containing byproduct recovery system is related to.

Background

In the production process of fluorine-containing fine chemical products, more side products are generated due to more chemical side reactions. In the production process, after a main product at the tail end is extracted, more other mixtures (containing organic auxiliary agents, fluorine-containing byproducts and other substances) remain, if the mixtures are not recycled in time by taking measures, certain safety and environmental protection risks exist, meanwhile, the waste of raw material consumption is caused, the manufacturing cost of the product is increased, and the disposal cost of waste is increased.

SUMMERY OF THE UTILITY MODEL

The utility model discloses a solve among the prior art problem of the recovery processing of other mixtures in fluorine-containing fine chemicals production process, provide a fluorine-containing by-product recovery system, through collect the by-product mixture, alkali lye washes water washing, washing mixture sedimentation separation, washing liquid rectification separation, deposit distillation separation and condensation realize the recovery of organic auxiliary agent and fluorine-containing by-product.

The utility model adopts the technical proposal that:

a fluorine-containing byproduct recovery system comprising:

a mixture wash column having a feed inlet and a water inlet;

the mixture washing water settling tank is communicated with a liquid outlet of the mixture washing tower;

the sediment rectifying tower is communicated with a liquid outlet of the mixture washing water settling tank;

the first refrigerant heat exchanger is communicated with an outlet of the sediment rectifying tower;

the rectification byproduct storage tank is communicated with an outlet of the first refrigerant heat exchanger;

a kettle bottom product collecting tank which is communicated with a bottom outlet of the sediment rectifying tower;

the organic auxiliary agent rectifying tower is communicated with the mixture washing water settling tank;

the second refrigerant heat exchanger is communicated with the organic auxiliary agent rectifying tower;

the organic auxiliary agent recovery storage tank is communicated with the second refrigerant heat exchanger; and

the residue collecting tank is communicated with the organic auxiliary agent rectifying tower;

wherein, the feed inlet is communicated with a conveying pipe of fluorine-containing byproducts, and the water inlet is communicated with a conveying pipe of alkali washing water.

Optionally, the mixture wash water settling tank comprises:

the bottom of the tank body is provided with a sediment outlet communicated with the sediment rectifying tower;

the groove cover is arranged at the notch of the groove body, and a mounting hole is formed in the groove cover;

one end of the liquid inlet pipeline is connected into the mounting hole, and the other end of the liquid inlet pipeline is communicated with a liquid outlet of the mixture washing tower;

the stirring devices are uniformly arranged on the inner side wall of the tank body;

and one end of the conveying pipeline is positioned in the tank body, and the other end of the conveying pipeline is connected into the organic auxiliary agent rectifying tower.

Optionally, the bottom of the tank body is arc-shaped or trumpet-shaped, and the sediment outlet is located at the lowest position of the bottom of the tank body.

Optionally, the mixture wash water settling tank further comprises:

and the pressurizing mechanism is communicated with the interior of the groove body.

Optionally, a plurality of agitating unit evenly distributed along the axis direction of cell body, agitating unit includes:

the stirring shaft is arranged on the side wall of the tank body, one end of the stirring shaft extends into the tank body, and the other end of the stirring shaft is positioned outside the tank body;

the stirring blades are spirally arranged on the stirring shaft in the tank body;

and the power output end of the driving motor is connected with the stirring shaft positioned outside the tank body.

Optionally, the outer sides of the stirring shaft and the stirring blades are wrapped with a protective layer.

Optionally, the protective layer is an anticorrosive layer formed by coating anticorrosive paint on the stirring shaft and the stirring blades and then solidifying the anticorrosive paint.

Optionally, the outer side wall of one end of the conveying pipeline, which is located on the trough body, is provided with a plurality of liquid inlet holes communicated with the inside of the conveying pipeline along the axis direction.

Compared with the prior art, the beneficial effects of the utility model are that:

collecting a byproduct mixture separated after the final product is extracted by a mixture washing tower, washing the byproduct mixture in the mixture washing tower by using alkali washing water, performing sedimentation separation on the washed mixture, performing rectification separation on the washing clear liquid, recycling the extracted organic auxiliary agent, and performing waste treatment on the distillate liquid; simultaneously, the separated sediment is subjected to distillation separation, and the gas-phase fluorine-containing organic matter is condensed by the distillate and is respectively collected with the fluorine-containing kettle bottom fraction to be sold as a product; by adopting the method, the organic auxiliary agents of tertiary butanol, fluorine-containing olefin and residual products in the byproduct mixture can be recycled or sold as products, on one hand, the production cost can be greatly reduced; on the other hand, the production of wastes is reduced, and the environment-friendly clean production is promoted.

Drawings

In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a schematic view of the overall flow structure of a fluorine-containing byproduct recovery system.

FIG. 2 is a schematic diagram showing the structure of a mixture wash water settling tank of the fluorine-containing byproduct recovery system.

FIG. 3 is a schematic diagram of a fluorine-containing byproduct recovery system having a caustic neutralization line.

FIG. 4 is a schematic diagram of a fluorine-containing byproduct recovery system having a transfer line.

Reference numerals:

1. a mixture washing column; 2. a mixture washing water settling tank; 21. a trough body; 22. a slot cover; 23. mounting holes; 24. a liquid inlet pipeline; 25. a stirring device; 251. a stirring shaft; 252. a stirring blade; 253. a drive motor; 26. a delivery conduit; 27. a pressurizing mechanism; 28. a sediment outlet; 29. a delivery conduit; 3. a sediment rectification column; 4. a first refrigerant heat exchanger; 5. a product collecting tank at the bottom of the kettle; 6. an organic auxiliary agent rectifying tower; 7. a second refrigerant heat exchanger; 8. an organic auxiliary agent recovery storage tank; 9. an additive mixing conduit; 91. a liquid discharge conduit; 92. a pump; 93. a mixing duct; 94. an additive liquid inlet pipe; 95. a liquid delivery pipeline; 10. a rectification byproduct storage tank; 110. and a residue collecting tank.

Detailed Description

In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.

In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings, or are orientations and positional relationships conventionally understood by those skilled in the art, which are merely for convenience of description and simplicity of description, and are not intended to indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the invention.

In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally formed; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.

The following disclosure provides many different embodiments or examples for implementing different features of the invention. In order to simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or reference letters in the various examples, which have been repeated for purposes of simplicity and clarity and do not in themselves dictate a relationship between the various embodiments and/or arrangements discussed.

Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

As shown in fig. 1 and 4, an embodiment of the present invention provides a fluorine-containing byproduct recovery system, including: the device comprises a mixture washing tower 1, a mixture washing water settling tank 2, a sediment rectifying tower 3, a first refrigerant heat exchanger 4, a rectifying byproduct storage tank 10, a kettle bottom product collecting tank 5, an organic auxiliary rectifying tower 6, a second refrigerant heat exchanger 7, an organic auxiliary recovery storage tank 8 and a residue collecting tank 110;

the mixture washing tower 1 is provided with a feed inlet and a water inlet; the mixture washing water settling tank 2 is communicated with a liquid outlet of the mixture washing tower 1; the sediment rectifying tower 3 is communicated with a liquid outlet of the mixture washing water settling tank 2, and the sediment rectifying tower 3 is provided with a steam inlet, a condensed water outlet and a rectified matter collecting port; the first refrigerant heat exchanger 4 is communicated with an outlet of the sediment rectifying tower 3; the rectification byproduct storage tank 10 is communicated with an outlet of the first refrigerant heat exchanger 4; the kettle bottom product collecting tank 5 is communicated with a rectification object collecting port of the sediment rectification tower 3; the organic auxiliary agent rectifying tower 6 is communicated with the mixture washing water settling tank 2 and is provided with a steam inlet, a condensed water outlet and a residue collecting port; the second refrigerant heat exchanger 7 is communicated with the organic auxiliary agent rectifying tower 6, a steam inlet, a condensed water outlet and a residue outlet are arranged on the organic auxiliary agent rectifying tower 6, a residue collecting tank 110 is arranged corresponding to the residue outlet, and after rectification is carried out; the organic auxiliary agent recovery storage tank 8 is communicated with the second refrigerant heat exchanger 7; wherein, the feed inlet is communicated with a conveying pipe of fluorine-containing byproducts, and the water inlet is communicated with a conveying pipe of alkali washing water.

When the device is used, a byproduct mixture separated after a final product is extracted is collected by the mixture washing tower 1, then the mixture is washed in the mixture washing tower 1 by alkali wash water, the washed mixture enters the mixture wash water settling tank 2 for settling separation, clear liquid of the settled washing liquid enters the organic auxiliary agent rectifying tower 6 for rectifying separation, the extracted organic auxiliary agent is recycled to the system, and the distillate liquid is subjected to waste treatment; simultaneously, the separated sediment is subjected to distillation separation, fluorine-containing organic matters are recovered after distillation and condensation and are sold as products, and distillate at the bottom of the kettle is collected and is treated as waste; by adopting the method, the organic auxiliary agents of tertiary butanol, fluorine-containing olefin and products in the byproduct mixture can be recycled or sold as products, on one hand, the production cost can be greatly reduced; on the other hand, the production of wastes is reduced, and the environment-friendly clean production is promoted. Wherein the arrows in figure 1 point in the direction of transport of the material.

In another embodiment, as shown in fig. 2 and 4, the mixture wash water settling tank 2 includes: the device comprises a tank body 21, a tank cover 22, a liquid inlet pipeline 24, a plurality of stirring devices 25 and a conveying pipeline 29; the bottom of the tank 21 is provided with a sediment outlet 28 communicated with the sediment rectification tower 3; the groove cover 22 is arranged at the notch of the groove body 21, and the groove cover 22 is provided with a mounting hole 23; one end of a liquid inlet pipeline 24 is connected into the mounting hole 23, and the other end of the liquid inlet pipeline is communicated with a liquid outlet of the mixture washing tower 1 and extends to a position where the middle part of the groove body 21 faces downwards; the stirring devices 25 are uniformly arranged on the inner side wall of the tank body 21; one end of the conveying pipeline 29 is positioned in the groove body 21, and the other end is connected to the organic auxiliary agent rectifying tower 6.

The mixture washed by the mixture washing tower 1 enters the tank body 21 for precipitation, is fully mixed by the stirring device 25 after entering the tank body 21, is precipitated for a period of time after mixing, is subjected to solid-liquid separation, is discharged into the organic auxiliary agent rectifying tower 6 for rectification by the liquid through the conveying pipeline 29, and is discharged into the sediment rectifying tower 3 for rectification.

In another embodiment, as shown in fig. 2, in order to facilitate the discharge of the sediment out of the tank 21, the bottom of the tank 21 is curved or flared, and the sediment outlet 28 is located at the lowest position of the bottom of the tank 21.

In another embodiment, as shown in fig. 2, in order to further facilitate the discharge of the precipitate, the mixture wash water settling tank 2 further comprises: and a pressurizing mechanism 27, wherein the pressurizing mechanism 27 is communicated with the inside of the groove body 21. The pressurizing mechanism 27 in this embodiment is an existing pneumatic pressurizing mechanism, and discharges the sediment in the tank 21 into the sediment rectification column 3 quickly by utilizing the difference between the pressures inside and outside the tank 21.

In another embodiment, as shown in fig. 2 and 3, in order to more sufficiently mix the mixture entering the tank 21 quickly, a plurality of stirring devices 25 are uniformly distributed along the axial direction of the tank 21, and each stirring device 25 includes: the stirring shaft 251, the stirring blade 252 and the driving motor 253, wherein the stirring shaft 251 is installed on the side wall of the tank body 21, one end of the stirring shaft 251 extends into the tank body 21, and the other end of the stirring shaft is positioned at the outer side of the tank body 21; the stirring blade 252 is spirally arranged on the stirring shaft 251 positioned in the tank body 21; the power output end of the driving motor 253 is connected with the stirring shaft 251 positioned outside the groove body 21.

The driving motor 253 drives the stirring shaft 251 to rotate, and the stirring blade 252 on the stirring shaft 251 drives the mixture to move, so that the mixture is left to stand and precipitate after being mixed in the tank 21. A plurality of agitating unit 25 are along the tank bottom lateral wall evenly installed of cell body 21, stir through a plurality of agitating unit 25 of even setting, because the solid in the mixture keeps away from the stirring power that the decline makes the required stirring power in cell body 21 bottom be greater than the supernatant because of gravity, consequently sets up this agitating unit 25 and is lieing in the bottom that the cell body is 21, and the mixture of bottom drives the liquid of upper portion under the effect of stirring power and carries out mixing motion.

In another embodiment, as shown in fig. 2, in order to facilitate discharging the precipitated phase washing water into the organic auxiliary agent rectification column 6, a drainage mechanism 26 is provided on the tank cover 22, and the drainage mechanism 26 includes: a drainage pipe 261 and a suction pump 262, wherein one end of the drainage pipe 261 penetrates through the trough cover 22 and extends to the interior of the trough body 21, and the other end of the drainage pipe 261 is communicated with the organic auxiliary agent rectifying tower 6; a suction pump 262 is installed on the drain tube 261.

In another embodiment, in order to improve the service life of the stirring shaft 251 and the stirring blades 252, the outer sides of the stirring shaft 251 and the stirring blades 252 are covered with a protective layer. The protective layer is an anticorrosive layer, and is coated on the stirring shaft 251 and the stirring blade 252 through anticorrosive paint, and the protective layer is formed after the anticorrosive paint is solidified.

In another embodiment, as shown in fig. 2, in order to facilitate discharging the supernatant after the precipitation, a plurality of liquid inlet holes communicated with the inside of the conveying pipe 29 are formed on the outer side wall of one end of the trough body 21 of the conveying pipe 29 along the axial direction thereof. The liquid inlet of the conveying pipeline 29 is prevented from being blocked by the sediment of the mixture, so that the liquid cannot be discharged into the organic auxiliary agent rectifying tower 6 through the conveying pipeline 29; and meanwhile, the plurality of liquid inlet holes are formed in the side wall along the axial direction of the organic auxiliary agent rectifying tower, so that the phenomenon that supernatant liquid cannot be conveyed into the organic auxiliary agent rectifying tower 6 due to blockage of part of the liquid inlet holes by sediments is further avoided.

In another embodiment, as shown in fig. 2, in order to increase the discharging efficiency of the supernatant, the liquid inlet holes are arranged in a row along the axial direction of the conveying pipe 29, and a plurality of groups of liquid inlet holes arranged in a row are circumferentially arranged on the conveying pipe 29, so that the reduction of the discharging efficiency of the supernatant caused by the blockage of part of the liquid inlet holes is avoided.

In another embodiment, as shown in fig. 3, an additive mixing pipeline 9 is provided between the mixture wash settling tank 2 and the organic auxiliary rectification column 6 for adding an additive to the phase-soluble wash water.

In another embodiment, the additive mixing pipe 9 includes, for convenience of mixing with an additive during the delivery of the phase-soluble washing water: a liquid discharge pipeline 91, a pump 92, a mixing pipeline 93, an additive liquid inlet pipe 94 and a liquid delivery pipeline 95; one end of the liquid discharge pipe 91 extends into the mixture washing water settling tank 2; a pump 92 is mounted on the drain pipe 91; a mixing pipe 93 is connected with the other end of the liquid discharge pipe 91; an additive liquid inlet pipe 94 is connected to the mixing pipeline 93, one end of a liquid feeding pipeline 95 is connected with the other end of the mixing pipeline 93, and the other end of the liquid feeding pipeline is connected with the organic auxiliary agent rectifying tower 6; the mixing pipeline 93 is spirally arranged, and the additive liquid inlet pipe 94 is connected to a liquid inlet end of the mixing pipeline 93.

When the device is used, the pump 92 extracts the precipitated phase soluble washing water from the mixture washing tower 1, the phase soluble washing water enters the spiral mixing pipeline 93 to be mixed with the additive entering through the additive liquid inlet pipe 94, and the mixed liquid is sent into the organic auxiliary agent rectifying tower 6 through the liquid feeding pipeline 95 to be rectified. More specifically, the mixing pipe 93 is spirally disposed, so that the mutually soluble washing water and the additive entering the mixing pipe 93 can be mixed sufficiently.

The specific working principle is as follows:

in view of the above situation, we firstly conducted an analysis study on a byproduct mixture through a test (the mixture contains about 35% of organic auxiliary agent tert-butyl alcohol, fluorine-containing byproducts (fluorine-containing olefin and other fluorine-containing impurities account for about 55%, acrylic acid and other about 10%), and then extracted and utilized in a combined manner of washing, neutralization and rectification according to different physical properties (such as water solubility, i.e., tert-butyl alcohol and acrylic acid are easily dissolved in water, and boiling points of materials in the mixture) of each substance in the byproduct mixture, thereby realizing comprehensive utilization of the byproducts.

Firstly, collecting the mixture of the byproducts in a mixture washing tower 1, then introducing 10% of alkaline washing water for washing, dissolving water-soluble organic auxiliary agents such as tert-butyl alcohol, acrylic acid and the like which are soluble in water into water, and then discharging the washed mixture which is soluble in water and is not soluble in water and the mixture which is insoluble in water into a mixture washing water settling tank 2 for settling separation by utilizing the difference between the specific gravity (about 1.0-1.1) of the mixture of the washing water dissolved in water and the specific gravity (about 1.6-1.7) of other mixtures (fluorine-containing byproducts, fluorine-containing olefin and other fluorine-containing impurities) which are insoluble in water.

Firstly, collecting the phase washing water (containing organic auxiliary agents such as tert-butyl alcohol and acrylic acid dissolved in water) after sedimentation separation, conveying the collected phase washing water to an organic auxiliary agent rectifying tower 6 through a conveying pipeline for stepwise rectification, collecting a light component organic solvent tert-butyl alcohol after rectification and concentration, using the light component organic solvent tert-butyl alcohol as a production auxiliary material and returning the light component organic solvent to a production system for utilization, and collecting the rest rectifying kettle bottom material for waste treatment; after being collected, the mixture of the fluorine-containing byproducts (including fluorine-containing olefin and other fluorine-containing substances) which are washed, settled and separated and are insoluble in water is sent into a sediment rectifying tower 3 for rectification, the fluorine-containing olefin can be taken as a light component and is taken out at the top of the rectifying tower for qualified analysis, and then the light component is collected as a general market product after being condensed by a first condenser. Finally collecting the rectified kettle bottom materials (the rest other fluorine-containing mixed materials) as waste to be treated by an environmental protection qualification unit.

In another embodiment, firstly, collecting the phase washing water (containing organic auxiliary agents such as tert-butyl alcohol and acrylic acid dissolved in water) after sedimentation separation, neutralizing the collected phase washing water in an alkali liquor neutralization pipeline 9, pumping the washing liquid after alkali liquor neutralization into an organic auxiliary agent rectifying tower 6 for stepwise rectification, collecting the light component organic solvent tert-butyl alcohol after rectification and concentration, and returning the light component organic solvent tert-butyl alcohol to a production system for utilization as a production auxiliary material, and collecting the rest rectifying still bottom material for waste treatment; after being collected, the mixture of the fluorine-containing byproducts (including fluorine-containing olefin and other fluorine-containing substances) which are washed, settled and separated and are insoluble in water is sent into a sediment rectifying tower 3 for rectification, the fluorine-containing olefin can be taken as a light component and is taken out at the top of the rectifying tower for qualified analysis, and then the light component is collected as a general market product after being condensed by a first condenser. Finally collecting the rectified kettle bottom materials (the rest other fluorine-containing mixed materials) as waste to be treated by an environmental protection qualification unit.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A fluorine-containing byproduct recovery system, comprising:

a mixture wash column having a feed inlet and a water inlet;

the sediment rectifying tower is communicated with the liquid outlet of the mixture washing water settling tank;

a kettle bottom product collecting tank which is communicated with an outlet at the bottom of the sediment rectification tower;

2. The fluorine-containing byproduct recovery system of claim 1 wherein the mixture wash water settling tank comprises:

the groove cover is arranged at the notch of the groove body, and is provided with a mounting hole;

3. The fluorine-containing byproduct recovery system according to claim 2, wherein the bottom of the tank body is arc-shaped or trumpet-shaped, and the sediment outlet is located at the lowest position of the bottom of the tank body.

4. The fluorine-containing byproduct recovery system of claim 3, wherein the mixture wash water settling tank further comprises:

5. The fluorine-containing byproduct recovery system according to claim 2, wherein a plurality of the stirring devices are uniformly distributed along an axial direction of the tank body, and the stirring devices comprise:

6. The fluorine-containing byproduct recovery system according to claim 5, wherein the stirring shaft and the outer side of the stirring blade are covered with a protective layer.

7. The fluorine-containing byproduct recycling system according to claim 6, wherein the protective layer is an anticorrosive layer formed by coating anticorrosive paint on the stirring shaft and the stirring blades and then solidifying the anticorrosive paint.

8. The system for recovering fluorine-containing byproducts according to claim 2, wherein the conveying pipeline is provided with a plurality of liquid inlet holes which are communicated with the inside of the conveying pipeline along the axial direction of the conveying pipeline and are positioned on the outer side wall of one end of the tank body.