CN114713294B - A treatment system and method for waste antimony pentachloride catalyst - Google Patents
A treatment system and method for waste antimony pentachloride catalyst Download PDFInfo
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- CN114713294B CN114713294B CN202110012627.9A CN202110012627A CN114713294B CN 114713294 B CN114713294 B CN 114713294B CN 202110012627 A CN202110012627 A CN 202110012627A CN 114713294 B CN114713294 B CN 114713294B
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- catalyst
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- 239000002699 waste material Substances 0.000 title claims abstract description 36
- 239000003054 catalyst Substances 0.000 title claims abstract description 32
- VMPVEPPRYRXYNP-UHFFFAOYSA-I antimony(5+);pentachloride Chemical compound Cl[Sb](Cl)(Cl)(Cl)Cl VMPVEPPRYRXYNP-UHFFFAOYSA-I 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 53
- 230000007062 hydrolysis Effects 0.000 claims abstract description 44
- 239000003513 alkali Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000007790 solid phase Substances 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- VOPWNXZWBYDODV-UHFFFAOYSA-N Chlorodifluoromethane Chemical compound FC(F)Cl VOPWNXZWBYDODV-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims abstract description 3
- 239000007800 oxidant agent Substances 0.000 claims abstract description 3
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 9
- 238000005336 cracking Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000008235 industrial water Substances 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims 2
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002912 waste gas Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- RWRIWBAIICGTTQ-UHFFFAOYSA-N difluoromethane Chemical compound FCF RWRIWBAIICGTTQ-UHFFFAOYSA-N 0.000 description 6
- 238000000197 pyrolysis Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 239000003518 caustics Substances 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 235000011837 pasties Nutrition 0.000 description 3
- 229910021630 Antimony pentafluoride Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- VBVBHWZYQGJZLR-UHFFFAOYSA-I antimony pentafluoride Chemical compound F[Sb](F)(F)(F)F VBVBHWZYQGJZLR-UHFFFAOYSA-I 0.000 description 2
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/64—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using alkaline material; using salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
本发明涉及废催化剂回收技术领域，具体涉及一种废五氯化锑催化剂的处理系统及处理方法。所述处理系统包括水解装置、离心装置、干燥装置；所述水解装置内设有搅拌装置，其顶部设有废催化剂进口、碱液进口、氧化剂进口和进水口，侧壁设有清液出口，底部设有浆液出口；所述水解装置的浆液出口与离心装置的入口相连；所述离心装置的固相出口与干燥装置的入口相连。该处理系统工艺流程简单，降低目前废催化剂处理的能耗成本，并且在碱性条件下水解反应，水解釜的材质无需耐酸，大大降低设备投资，同时具有密闭性、安全性、自动化程度高的优点，废水、废气均严格处理，达标排放，可在二氟一氯甲烷生产中得到广泛应用。
The present invention relates to the technical field of waste catalyst recovery, and specifically to a treatment system and method for waste antimony pentachloride catalyst. The treatment system comprises a hydrolysis device, a centrifugal device, and a drying device; the hydrolysis device is provided with a stirring device, and the top is provided with a waste catalyst inlet, an alkali liquid inlet, an oxidant inlet, and a water inlet, the side wall is provided with a clear liquid outlet, and the bottom is provided with a slurry outlet; the slurry outlet of the hydrolysis device is connected to the inlet of the centrifugal device; the solid phase outlet of the centrifugal device is connected to the inlet of the drying device. The treatment system has a simple process flow, reduces the energy consumption cost of the current waste catalyst treatment, and the hydrolysis reaction is carried out under alkaline conditions, and the material of the hydrolysis kettle does not need to be acid-resistant, which greatly reduces the equipment investment. At the same time, it has the advantages of airtightness, safety, and high degree of automation. Wastewater and waste gas are strictly treated and discharged up to the standard, and can be widely used in the production of difluoromonochloromethane.
Description
Technical Field
The invention relates to the technical field of waste catalyst recovery, in particular to a treatment system and a treatment method of a waste antimony pentachloride catalyst.
Background
The activity of the catalyst antimony pentachloride used in the production of the difluoro-chloromethane gradually decreases after a period of reaction until part of the catalyst loses activity to become antimony pentafluoride, so that part of the catalyst in the reaction kettle needs to be replaced after a period of reaction.
The waste antimony pentachloride catalyst contains chloroform, antimony pentachloride, antimony trichloride, antimony pentafluoride and other organic high-boiling substances, belongs to highly harmful substances, and generates a large amount of toxic and harmful gases in the hydrolysis process, and the existing treatment method has the disadvantages of long process flow, high energy consumption and high separation difficulty, and cannot meet the increasingly high requirements of society on automation, safety, environmental protection, energy conservation of chemical industry, environmental protection devices and the like.
Disclosure of Invention
Aiming at the problems, the invention provides a treatment system and a treatment method for waste antimony pentachloride catalyst in the production process of difluoromethane.
Specifically, the invention provides the following technical scheme:
a treatment system of waste antimony pentachloride catalyst comprises a hydrolysis device, a centrifugal device and a drying device;
The hydrolysis device is internally provided with a stirring device, the top of the hydrolysis device is provided with a spent 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;
the solid phase outlet of the centrifugal device is connected with the inlet of the drying device.
Preferably, in the above treatment system, the hydrolysis device is further provided with an exhaust port, the exhaust port of the hydrolysis device is connected with a water caustic washing system, and the water caustic washing system is used for treating acid gas by water caustic washing and collecting the acid gas.
Preferably, in the above treatment system, the clear liquid outlet of the hydrolysis device is connected to a spent caustic tank.
Preferably, in the above processing system, the centrifugal device is a horizontal scraper discharge centrifugal machine, 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 be blocked (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 pyrolysis device, and the liquid phase outlet of the centrifugal device is connected with the plasma pyrolysis device.
Preferably, in the above processing system, the drying device is provided with an exhaust port, and the exhaust port of the drying device is connected with the plasma pyrolysis device.
The invention also provides a treatment method of the waste antimony pentachloride catalyst, which comprises the following steps:
(1) Adding industrial water into a hydrolysis device, and further adding sodium hydroxide solution to adjust the pH value to be more than 10;
(2) Continuously adding a waste antimony pentachloride catalyst and hydrogen peroxide into the hydrolysis device respectively, keeping a certain temperature and stirring speed for hydrolysis reaction, and enabling 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 centrifugal machine 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 adding sodium hydroxide solution.
Preferably, in the above treatment method, the temperature of the hydrolysis reaction is 50 to 60 ℃.
Preferably, in the above 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 the molar flow ratio of Sb 3+ in the continuously added waste antimony pentachloride catalyst to the hydrogen peroxide is 1.8-2.2:3, preferably 2:3.
The beneficial effects obtained by the invention are as follows:
The treatment system of the waste antimony pentachloride catalyst provided by the invention has the advantages of simple process flow, reduced energy consumption cost of the existing waste catalyst treatment, no acid resistance of materials of a hydrolysis kettle, greatly reduced equipment investment, improved economic benefit and environmental benefit of enterprises, high tightness, safety and high degree of automation, and strict treatment of waste water and waste gas, standard emission, and wide application in difluoromethane production.
Drawings
FIG. 1 is a schematic diagram of the apparatus described in example 1, wherein 1, a hydrolysis kettle, 2, a horizontal scraper discharge centrifuge, 3, a double-cone rotary vacuum dryer, 4, a water alkali washing system, 5, a waste alkali tank, 6, a fluorine-containing wastewater treatment device, 7, and a plasma pyrolysis device.
Detailed Description
The following examples are illustrative of the invention and are not intended to limit the scope of the invention. The specific techniques or conditions are not identified in the examples and are described in the literature in this field or are carried out in accordance with the product specifications.
In the description of the present invention, unless otherwise indicated, the terms "upper," "lower," and the like refer to an orientation or state relationship based on that shown in the drawings, for convenience of description and simplicity of description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the invention.
In the following examples, the equipment and the like used were conventional products available for purchase by a regular channel manufacturer, without specifying the manufacturer. The methods are conventional methods unless otherwise specified, and the starting materials are commercially available from the public sources unless otherwise specified.
In the following examples, the waste antimony pentachloride used was derived from an F22 reactor, about 30% of the waste antimony pentachloride (the proportion of Sb3+ in the waste antimony pentachloride was about 20%), 60% of chloroform, 1% of hydrogen chloride, 4% of hydrogen fluoride, the balance F21 and the like.
Example 1
As shown in fig. 1, embodiment 1 provides a treatment system of waste antimony pentachloride catalyst in a difluoromethane 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;
the hydrolysis kettle 1 is internally provided with a stirring device, the top of the hydrolysis kettle is provided with a waste antimony pentachloride catalyst inlet, a sodium hydroxide solution inlet, a hydrogen peroxide solution 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 a water alkali washing system 4;
the 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 centrifugal machine 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 dryer 3, and the liquid phase outlet is connected with the plasma pyrolysis device 7;
The bipyramid gyration vacuum dryer 3 is equipped with the gas vent, and this gas vent is connected with the plasma pyrolysis 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:
2000kg of industrial water is added into a hydrolysis kettle 1 (made of carbon steel, V=5m 3), 15r/min stirring is started, about 400kg of 15% sodium hydroxide aqueous solution is prepared and added into 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 a rate of 300kg/h through a level difference, hydrogen peroxide is added at a rate of 1m 3/h while the waste antimony pentachloride catalyst is added, the pH value is automatically monitored, and if the pH value is reduced to 10, 0.1m 3 of 15% sodium hydroxide aqueous solution is automatically added, so that the solution in the hydrolysis kettle is always alkaline. After the addition, the stirring is closed, the mixture is cooled to normal temperature, and acid gases such as HF, HCl and the like generated in the hydrolysis process enter a water alkali washing system 4 for treatment and then are discharged after reaching standards.
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 pasty substances, organic phases and a small amount of inorganic phases enter a horizontal scraper discharge centrifuge 2, the pasty substances are separated out at the rotating speed of 3500-5000 r/min, the organic phases and the small amount of inorganic phases are conveyed to a plasma cracking device 7 for treatment, the pasty substances are conveyed to a double-cone rotary vacuum dryer 3 for micro-negative pressure and drying at 120-150 ℃ to obtain a finished product (about 60kg, and the antimony pentoxide content is about 60-70%), and the dried waste gas is conveyed to the ion cracking device 7 for treatment.
While the invention has been described in detail in the foregoing general description, embodiments and experiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (10)
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| CN202110012627.9A CN114713294B (en) | 2021-01-06 | 2021-01-06 | A treatment system and method for waste antimony pentachloride catalyst |
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| CN114713294B true CN114713294B (en) | 2025-01-07 |
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