CN114713294A - Treatment system and treatment method of waste antimony pentachloride catalyst - Google Patents
Treatment system and treatment method of waste antimony pentachloride catalyst Download PDFInfo
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- CN114713294A CN114713294A CN202110012627.9A CN202110012627A CN114713294A CN 114713294 A CN114713294 A CN 114713294A CN 202110012627 A CN202110012627 A CN 202110012627A CN 114713294 A CN114713294 A CN 114713294A
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- antimony pentachloride
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- 239000002699 waste material Substances 0.000 title claims abstract description 40
- 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 28
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 59
- 230000007062 hydrolysis Effects 0.000 claims abstract description 49
- 239000003513 alkali Substances 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000007790 solid phase Substances 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 5
- 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 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- 238000005336 cracking Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 11
- 238000012545 processing Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 239000008235 industrial water Substances 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 230000001502 supplementing effect Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 3
- 239000003518 caustics Substances 0.000 claims 1
- VOPWNXZWBYDODV-UHFFFAOYSA-N Chlorodifluoromethane Chemical compound FC(F)Cl VOPWNXZWBYDODV-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 5
- 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
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 3
- 229910000040 hydrogen fluoride Inorganic materials 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
- 230000002378 acidificating effect Effects 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
- 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
- 238000001816 cooling Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 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
Images
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
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- 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
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. 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 the advantages of simple process flow, reduction of energy consumption cost of the treatment of the existing waste catalyst, hydrolysis reaction under an alkaline condition, no need of acid resistance of the material of the hydrolysis kettle, great reduction of equipment investment, high tightness, safety and automation degree, strict treatment of wastewater and waste gas, standard discharge and wide application in the production of the difluorochloromethane.
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 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.
Disclosure of Invention
Aiming at the problems, the invention provides a system and a method for treating a waste antimony pentachloride catalyst in a chlorodifluoromethane production process.
Specifically, the invention provides the 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 acidic 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 invention also provides a method for treating the waste antimony pentachloride catalyst, which comprises the following steps:
(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 invention has the following beneficial effects:
the system for treating the waste antimony pentachloride catalyst provided by the invention has a simple process flow, reduces the energy consumption cost of the prior waste catalyst treatment, performs hydrolysis reaction under an alkaline condition, does not need acid resistance due to the material of a hydrolysis kettle, and greatly reduces the equipment investment, so that the economic benefit and the environmental benefit of enterprises are improved.
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 those shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element 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.
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, starting stirring at 15r/min, preparing about 400kg of 15% sodium hydroxide aqueous solution, adding the 15% sodium hydroxide aqueous solution into a hydrolysis kettle 1, opening cooling circulating water in a jacket on the side wall of the hydrolysis kettle 1, slowly adding 600kg of waste antimony pentachloride catalyst into the hydrolysis kettle at the speed of 300kg/h through a potential difference, and adding the waste antimony pentachloride catalyst while adding the waste antimony pentachloride catalyst at the speed 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 10315% sodium hydroxide solutionAnd (4) 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 hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
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.
8. A treatment method of a waste antimony pentachloride catalyst is characterized by comprising the following steps:
(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.
9. The process according to claim 8, wherein the temperature of the hydrolysis reaction is 50 to 60 ℃.
10. The treatment method according to claim 8 or 9, wherein 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.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110012627.9A CN114713294A (en) | 2021-01-06 | 2021-01-06 | Treatment system and treatment method of waste antimony pentachloride catalyst |
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| CN202110012627.9A CN114713294A (en) | 2021-01-06 | 2021-01-06 | Treatment system and treatment method of waste antimony pentachloride catalyst |
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