CN214974063U - Processing system of useless antimony pentachloride catalyst - Google Patents
Processing system of useless antimony pentachloride catalyst Download PDFInfo
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- CN214974063U CN214974063U CN202120027086.2U CN202120027086U CN214974063U CN 214974063 U CN214974063 U CN 214974063U CN 202120027086 U CN202120027086 U CN 202120027086U CN 214974063 U CN214974063 U CN 214974063U
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Abstract
The utility model relates to a technical field, concretely relates to processing system of useless antimony pentachloride catalyst are retrieved to useless catalyst. The treatment system comprises a hydrolysis device, a centrifugal device and a drying device; a stirring device is arranged in the hydrolysis device, the top of the hydrolysis device is provided with a waste catalyst inlet, an alkali liquor inlet, an oxidant inlet and a water inlet, the side wall of the hydrolysis device is provided with a clear liquid outlet, and the bottom of the hydrolysis device is provided with a slurry outlet; the slurry outlet of the hydrolysis device is connected with the inlet of the centrifugal device; and the solid phase outlet of the centrifugal device is connected with the inlet of the drying device. The treatment system has simple process flow, reduces the energy consumption cost of the prior waste catalyst treatment, performs hydrolysis reaction under the alkaline condition, has no need of acid resistance for the material of a hydrolysis kettle, greatly reduces the equipment investment, has the advantages of high tightness, safety and automation degree, strictly treats waste water and waste gas, reaches the standard and is discharged, and can be widely applied to the production of the difluorochloromethane.
Description
Technical Field
The utility model relates to a technical field, concretely relates to processing system of useless antimony pentachloride catalyst are retrieved to useless catalyst.
Background
The activity of antimony pentachloride used in the production of chlorodifluoromethane is gradually reduced after a period of reaction until part of the catalyst loses activity and becomes antimony pentafluoride, so that part of the catalyst in the reaction kettle needs to be replaced after a period of time.
The waste antimony pentachloride catalyst contains organic high-boiling substances such as chloroform, antimony pentachloride, antimony trichloride, antimony pentafluoride and the like, belongs to highly harmful substances, and can generate a large amount of toxic and harmful gases in the hydrolysis process.
SUMMERY OF THE UTILITY MODEL
To the problem, the utility model provides a processing system of useless antimony pentachloride catalyst in difluoro chloromethane production process.
Particularly, the utility model provides a following technical scheme:
a processing system of a waste antimony pentachloride catalyst comprises a hydrolysis device, a centrifugal device and a drying device;
a stirring device is arranged in the hydrolysis device, the top of the hydrolysis device is provided with a waste catalyst inlet, an alkali liquor inlet, an oxidant inlet and a water inlet, the side wall of the hydrolysis device is provided with a clear liquid outlet, and the bottom of the hydrolysis device is provided with a slurry outlet;
the slurry outlet of the hydrolysis device is connected with the inlet of the centrifugal device;
and the solid phase outlet of the centrifugal device is connected with the inlet of the drying device.
Preferably, in the treatment system, the hydrolysis device is further provided with an exhaust port, the exhaust port of the hydrolysis device is connected with a water alkali washing system, and the water alkali washing system is used for treating and collecting acid gas by water alkali washing.
Preferably, in the above treatment system, the clear liquid outlet of the hydrolysis device is connected to the waste alkali tank.
Preferably, in the processing system, the centrifugal device is a horizontal scraper discharge centrifuge, and the drying device is a double-cone rotary vacuum dryer. After hydrolysis, a horizontal scraper discharge centrifuge and a double-cone rotary vacuum dryer are adopted for post-treatment, the whole system is not easy to block (sodium fluoride, sodium chloride and the like are easy to crystallize), and the drying efficiency is high.
Preferably, the treatment system further comprises a plasma cracking device, and the liquid phase outlet of the centrifugal device is connected with the plasma cracking device.
Preferably, in the processing system, the drying device is provided with an exhaust port, and the exhaust port of the drying device is connected with the plasma cracking device.
The utility model also provides a processing method of useless antimony pentachloride catalyst, including following step:
(1) adding industrial water into a hydrolysis device, and further adding a sodium hydroxide solution to adjust the pH value to be more than 10;
(2) respectively and continuously adding the waste antimony pentachloride catalyst and hydrogen peroxide into the hydrolysis device, keeping a certain temperature and stirring speed for hydrolysis reaction, and allowing acid gas generated in the reaction to enter a water alkali washing system for water alkali washing treatment;
(3) standing the feed liquid after the hydrolysis reaction, separating clear liquid from slurry, allowing the clear liquid to enter a waste alkali tank, allowing the slurry to enter a centrifuge for solid-liquid separation, allowing the separated liquid phase to enter a plasma cracking device, and allowing the separated solid phase to enter a dryer for drying treatment;
wherein, in the hydrolysis reaction, the pH value of the reaction system is kept above 10 by supplementing sodium hydroxide solution.
Preferably, in the above treatment method, the temperature of the hydrolysis reaction is 50 to 60 ℃.
Preferably, in the treatment method, the mass ratio of the total addition amount of the waste antimony pentachloride catalyst to the industrial water is 1-5: 10;
and/or Sb in the waste antimony pentachloride catalyst added continuously3+The molar flow ratio of the hydrogen peroxide to the hydrogen peroxide is 1.8-2.2: 3, and preferably 2: 3.
The utility model discloses the beneficial effect who gains:
the utility model provides a processing system of useless antimony pentachloride catalyst, process flow is simple, reduces the energy consumption cost that present useless catalyst handled, and hydrolysis reaction under alkaline condition, the material of cauldron of hydrolysising need not acid-fast, greatly reduced equipment investment, thereby improve the economic benefits and the environmental benefit of enterprise, have the advantage that seal, security, degree of automation are high simultaneously, waste water, waste gas all strictly handle, discharge to reach standard can obtain wide application in difluoro chloromethane production.
Drawings
FIG. 1 is a schematic view of the apparatus described in example 1; the device comprises a hydrolysis kettle 1, a horizontal scraper discharge centrifuge 2, a double-cone rotary vacuum dryer 3, a water alkali washing system 4, a waste alkali tank 5, a fluorine-containing wastewater treatment device 6 and a plasma cracking device 7.
Detailed Description
The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications.
In the description of the present invention, unless otherwise specified, the terms "upper", "lower", and the like indicate orientations or state relationships based on the orientations or state relationships shown in the drawings, and are only for convenience of description and simplified description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the following examples, the equipment and the like used are not shown to manufacturers, and are all conventional products available from regular vendors. The process is conventional unless otherwise specified, and the starting materials are commercially available from the open literature.
In the following examples, the used waste antimony pentachloride is from the F22 reaction kettle, about 30% of the waste antimony pentachloride (the ratio of Sb3+ in the waste antimony pentachloride is about 20%), 60% of chloroform, 1% of hydrogen chloride, 4% of hydrogen fluoride, and the balance of F21, etc.
Example 1
As shown in fig. 1, embodiment 1 provides a system for treating a waste antimony pentachloride catalyst in a monochlorodifluoromethane production process, which comprises a hydrolysis kettle 1, a horizontal scraper discharge centrifuge 2, a double-cone rotary vacuum dryer 3, a water alkali washing system 4, a waste alkali tank 5, a fluorine-containing wastewater treatment device 6 and a plasma cracking device 7;
a stirring device is arranged in the hydrolysis kettle 1, the top of the hydrolysis kettle is provided with a waste antimony pentachloride catalyst inlet, a sodium hydroxide solution inlet, a hydrogen peroxide inlet and an industrial water inlet, the side wall of the hydrolysis kettle is provided with a clear liquid outlet, and the bottom of the hydrolysis kettle is provided with a slurry outlet;
the hydrolysis kettle 1 is also provided with an exhaust port, and the exhaust port of the hydrolysis kettle 1 is connected with the water alkali washing system 4;
a clear liquid outlet of the hydrolysis kettle 1 is sequentially connected with a waste alkali tank 5 and a fluorine-containing wastewater treatment device 6;
the slurry outlet of the hydrolysis kettle 1 is connected with the inlet of a horizontal scraper discharge centrifuge 2;
the horizontal scraper discharging centrifuge 2 is provided with a solid phase outlet and a liquid phase outlet, the solid phase outlet is connected with the double-cone rotary vacuum drier 3, and the liquid phase outlet is connected with the plasma cracking device 7;
the double-cone rotary vacuum drier 3 is provided with an exhaust port which is connected with the plasma cracking device 7.
Example 2
The method for treating the waste antimony pentachloride catalyst by using the treatment system in the embodiment 1 comprises the following specific steps:
in a hydrolysis kettle 1 (made of carbon steel, V is 5m3) Adding 2000kg of industrial water, stirring at 15r/min, preparing about 400kg of 15% sodium hydroxide aqueous solution, and adding waterIn the hydrolysis kettle 1, cooling circulating water in a jacket on the side wall of the hydrolysis kettle 1 is opened, 600kg of waste antimony pentachloride catalyst is slowly added into the hydrolysis kettle at the speed of 300kg/h through a potential difference, and the waste antimony pentachloride catalyst is added and the added waste antimony pentachloride catalyst is added at the same time of 1m3Adding hydrogen peroxide at a speed of/h, automatically monitoring the pH value, and automatically supplementing 0.1m if the pH value is reduced to 103And 15% sodium hydroxide aqueous solution, so that the solution in the hydrolysis kettle is kept alkaline all the time. And after the feeding is finished, the stirring is closed, the mixture is cooled to normal temperature, and acidic gases such as HF (hydrogen fluoride), HCl and the like generated in the hydrolysis process enter a water alkali washing system 4 for treatment and then reach the standard to be discharged.
The upper inorganic clear liquid in the hydrolysis kettle 1 is discharged into a waste alkali tank 5 and then is conveyed to a fluorine-containing wastewater treatment device 6 through a pump; the rest of the slurry-like substance, the organic phase and a small amount of the inorganic phase enter a horizontal scraper discharge centrifuge 2, the slurry-like substance is separated at the rotating speed of 3500-5000 r/min, and the organic phase and the small amount of the inorganic phase are conveyed to a plasma cracking device 7 for treatment; the slurry material is conveyed into a double-cone rotary vacuum drier 3 to be dried under the micro negative pressure at the temperature of 120-150 ℃ to prepare a finished product (about 60kg, the content of antimony pentoxide is about 60-70%), and the dried waste gas is conveyed into an ion cracking device 7 to be treated.
Although the invention has been described in detail in the foregoing by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that certain modifications and improvements may be made thereto based on the invention. Therefore, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (7)
1. A processing system of a waste antimony pentachloride catalyst is characterized by comprising a hydrolysis device, a centrifugal device and a drying device;
a stirring device is arranged in the hydrolysis device, the top of the hydrolysis device is provided with a waste catalyst inlet, an alkali liquor inlet, an oxidant inlet and a water inlet, the side wall of the hydrolysis device is provided with a clear liquid outlet, and the bottom of the hydrolysis device is provided with a slurry outlet;
the slurry outlet of the hydrolysis device is connected with the inlet of the centrifugal device;
and the solid phase outlet of the centrifugal device is connected with the inlet of the drying device.
2. The treatment system according to claim 1, wherein the hydrolysis device is further provided with an exhaust port, the exhaust port of the hydrolysis device is connected with an aqueous alkaline cleaning system, and the aqueous alkaline cleaning system is used for treating and collecting acid gas by aqueous alkaline cleaning.
3. The treatment system of claim 1, wherein the clear liquid outlet of the hydrolysis apparatus is connected to a spent caustic tank.
4. The processing system of claim 1, wherein the centrifuge device is a horizontal knife discharge centrifuge.
5. The processing system of claim 1, wherein the drying device is a double-cone rotary vacuum dryer.
6. The processing system of claim 1, further comprising a plasma cracking unit, wherein the liquid phase outlet of the centrifuge is connected to the plasma cracking unit.
7. The processing system of claim 6, wherein the drying device is provided with an exhaust port, and the exhaust port of the drying device is connected to the plasma cracking device.
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| CN202120027086.2U CN214974063U (en) | 2021-01-06 | 2021-01-06 | Processing system of useless antimony pentachloride catalyst |
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| CN202120027086.2U CN214974063U (en) | 2021-01-06 | 2021-01-06 | Processing system of useless antimony pentachloride catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114713294A (en) * | 2021-01-06 | 2022-07-08 | 中昊晨光化工研究院有限公司 | Treatment system and treatment method of waste antimony pentachloride catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114713294A (en) * | 2021-01-06 | 2022-07-08 | 中昊晨光化工研究院有限公司 | Treatment system and treatment method of waste antimony pentachloride catalyst |
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