CN115155672A - Regeneration method of hydrogen chloride oxidation catalyst - Google Patents
Regeneration method of hydrogen chloride oxidation catalyst Download PDFInfo
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- CN115155672A CN115155672A CN202210728328.XA CN202210728328A CN115155672A CN 115155672 A CN115155672 A CN 115155672A CN 202210728328 A CN202210728328 A CN 202210728328A CN 115155672 A CN115155672 A CN 115155672A
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- 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
- B01J38/02—Heat treatment
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/90—Regeneration or reactivation
- B01J23/96—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the noble metals
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- 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
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
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- 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
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
- B01J38/10—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst using elemental hydrogen
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- 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
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
- B01J38/12—Treating with free oxygen-containing gas
- B01J38/14—Treating with free oxygen-containing gas with control of oxygen content in oxidation gas
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- 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
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
- B01J38/42—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst using halogen-containing material
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- 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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Abstract
The invention discloses a regeneration method of a hydrogen chloride oxidation catalyst, which comprises the steps of firstly treating the catalyst at 100-700 ℃ in a mixed atmosphere of reducing gas and inert gas; the reducing gas is H 2 、CH 3 I、CH 2 I 2 And CH 4 One or more of (a); the treated catalyst is calcined under the conditions of mixed gas flow of oxygen and inert gas and 100-700 ℃. The method can efficiently regenerate hydrogen chloride oxidation catalyst in situThe catalyst and regenerated catalyst have activity similar to that of fresh catalyst and similar service life and may be reused.
Description
Technical Field
The invention belongs to the field of catalyst preparation, and particularly relates to a high-efficiency regeneration method of a hydrogen chloride oxidation catalyst.
Background
As important basic chemicals, chlorine and hydrogen chloride have wide applications. Almost all chlorine-containing organic compounds are chlorine gas or liquid chlorine, and nearly 50% of chemical processes involve chlorine, and chlorine has a great importance in the chemical industry. However, in the field of chlorine-related industry, a large amount of byproduct hydrogen chloride is difficult to treat, and becomes one of the key bottlenecks for restricting the development of the chlorine-related industries such as polyurethane, pesticide, pharmaceutical chemical industry, fluorine chemical industry and the like.
Deacon in 1868 disclosed a method for preparing chlorine by catalytic oxidation of hydrogen chloride (US 85370), which is significant in recycling byproduct hydrogen chloride. A series of hydrogen chloride oxidation catalysts have been developed to date, and heterogeneous supported catalysts are mainly used, and the related active components comprise metal elements such as copper, iron, chromium, ruthenium, gold, cerium and the like, and the catalytic performances of the catalysts are different. Among them, ruthenium, which is a noble metal, has a relatively high catalytic oxidation activity of hydrogen chloride, and has been widely used for the catalytic oxidation recycling of industrial by-product hydrogen chloride, resulting in good industrial benefits. Among them, the highest Cl yield was achieved with ruthenium-based catalysts in the patent (US 6852667) 2 The space-time yield is 8.88X 10 -4 mol/(g cat Min), i.e. 3.78 g/(g) cat H). However, the noble metal ruthenium is expensive and is influenced by the demand in the field of electronic industry, and the price of ruthenium has been increasing rapidly in recent years. Therefore, the catalyst use cost is reduced, and the ruthenium base is treatedThe recycling of the catalyst has become an important research direction.
The deactivation mechanism of the ruthenium-based catalyst in the catalytic oxidation reaction of hydrogen chloride is mainly caused by sintering of a ruthenium active phase. The active phase of ruthenium mainly exists in the form of ruthenium oxide or oxychloride, and gradually migrates, ages and sinters on the surface of the carrier along with the prolonging of the reaction time, so that the active sites are reduced, and the overall activity of the catalyst is reduced.
Disclosure of Invention
In view of the defects or shortcomings of the prior art, the invention provides a regeneration method of a hydrogen chloride oxidation catalyst, which is used for regenerating a catalyst which takes ruthenium as an active component and is loaded on a carrier.
To this end, the method for regenerating a hydrogen chloride oxidation catalyst of the present invention comprises:
(1) Treating the catalyst in a mixed atmosphere of reducing gas and inert gas at 100-700 ℃; the reducing gas is H 2 、CH 3 I、CH 2 I 2 And CH 4 One or more of (a);
(2) Roasting the catalyst treated in the step (1) under the conditions of mixed gas flow of oxygen and inert gas and 100-700 ℃.
Alternatively, the regeneration process is carried out in situ in the reactor for the catalytic oxidation of hydrogen chloride.
Further, the active component is ruthenium oxide or ruthenium oxychloride.
Further, the carrier is rutile type titanium dioxide or anatase type titanium dioxide or a mixture of the rutile type titanium dioxide and the anatase type titanium dioxide. Furthermore, the mass fraction of anatase titanium dioxide in the mixture of the two is 10-60%.
Optionally, the step (1) is carried out at 200-500 ℃, and the step (2) is carried out at 200-400 ℃.
Optionally, the mixed gas of the reducing gas and the inert gas contains 20% to 100% of the reducing gas by volume fraction.
Optionally, the mixed gas of oxygen and inert gas contains 5-100% volume fraction of oxygen.
Optionally, the inert gas is nitrogen, helium or argon.
The invention also provides a method for preparing chlorine by catalytic oxidation of hydrogen chloride. The method for preparing the chlorine by the catalytic oxidation of the hydrogen chloride is characterized in that in the process of preparing the chlorine by the catalytic oxidation of the hydrogen chloride, the catalyst with reduced activity is not moved out of the reactor, and the catalyst is directly subjected to in-situ regeneration in the reactor by adopting the method, so that the chlorine is continuously prepared.
The invention promotes the redispersion of ruthenium active phase by reducing-reoxidizing the ruthenium-based catalyst with reduced activity, realizes the high-efficiency regeneration of the hydrogen chloride oxidation catalyst, and the activity of the regenerated catalyst can reach more than 90 percent of the activity of the fresh catalyst. Furthermore, the method can adopt a mode of regenerating the hydrogen chloride oxidation catalyst in situ, avoids the unloading and the secondary filling of the catalyst, is favorable for improving the industrial production efficiency and reducing the operation cost.
Detailed Description
Unless otherwise specified, the terminology herein is to be understood in light of the knowledge of one of ordinary skill in the relevant art.
The invention improves the dispersion property of ruthenium element by treating the catalyst with reduced activity in the atmosphere containing reducing gas, and then obtains the regenerated catalyst by oxidation treatment, thereby realizing the regeneration of the ruthenium-based catalyst which is partially deactivated. More preferably, the process of the invention can be regenerated in situ in the catalytic hydrogen chloride oxidation reactor. The catalyst with reduced activity is compared with a fresh catalyst, theoretically, the catalyst with reduced activity relative to the fresh catalyst can be regenerated by adopting the method, and in an actual scheme, a specific reduction standard can be selected according to the requirements of production cost, yield and the like.
The catalyst used in the method for preparing chlorine by catalytic oxidation of hydrogen chloride is a catalyst which takes ruthenium as an active component and is loaded on a carrier, and the specific preparation method is a preparation method known in the field.
On the basis of the scheme of the invention, the skilled person can optimally select the conditions involved in the method of the invention, including but not limited to the volume ratio of the reducing gas to the inert gas, the volume ratio of the oxygen to the inert gas, the reduction temperature, the oxidation temperature, and the like, so as to achieve the effects of the invention. The present invention is further illustrated by the following examples, but is not limited thereto.
The catalyst evaluation in the following examples employed a fixed bed reactor having dimensions of 420 mm. Times. Phi.20 mm. Times.5 mm. The reaction is carried out at atmospheric pressure, the catalyst being packed in 4.0. + -. 0.1g of cylindrical particles of 3X 3mm, with inert alpha-Al 2 O 3 Diluting with small ball (phi 3 mm); with HCl gas, O 2 The mixed gas is reaction gas, the flow rate of the reaction gas is controlled by a mass flow meter, the reaction gas enters a fixed bed reactor after passing through a preheater, the reactor is heated in three sections by adopting an electric heating mode, the reaction temperature is 350 ℃, the HCl flow rate is 480ml/min, and O is generated 2 The flow is 960ml/min, the sample is taken for analysis after the reaction is stable for 2h, and Cl in the sample is titrated by iodometry and acid-base titration respectively 2 And incompletely reacted HCl, the results of the analysis being used as initial catalytic activity data.
The specific operation steps are as follows: after the system is stably operated, preparing 100mL of 20% KI solution at regular intervals, switching an outlet three-way valve of an oxidation reactor, introducing the mixed gas after reaction into a constant volume (100 mL) potassium iodide solution, absorbing for 2 minutes, transferring the absorbing solution into a conical flask after absorption, titrating by using 0.1mol/L sodium thiosulfate standard solution, and using starch as an indicator; then, unreacted HC1 was titrated with 0.1mol/L sodium hydroxide standard solution using phenolphthalein as an indicator.
Because the conditions of higher reaction space velocity and temperature are adopted, the catalyst after 500h of reaction is taken as the catalyst to be regenerated, and the catalyst is evaluated under the same reaction conditions after regeneration.
Example 1:
the catalyst A1 of this example is: the mass fraction of Ru is 1.8%, the active component is ruthenium oxide, 0.7% of Si is added as a structural auxiliary agent, and the carrier is 80% of rutile TiO 2 And 20% anatase TiO 2 (ii) a Fresh catalyst realizes Cl 2 Space-time yield 6.18 g/(g) cat H) Cl after 500h 2 The space-time yield drops to 2.92 g/(g) cat ·h)；
The reaction gas circuit is closed and H is introduced 2 And N 2 Mixed gas (H) of 2 The volume fraction is 80 percent, and the rest is N 2 ) The flow rate is 100ml/min, the heating temperature is 300 ℃, and the heating time is kept for 1.5h; then close H 2 Gas path, holding N 2 Displacing for 10min, heating to 350 deg.C, and introducing 8ml/min O 2 And keeping for 3.0h to obtain a regenerated catalyst A2;
the catalyst A2 was re-evaluated under the same reaction conditions as described above, and the initial activity reached Cl 2 Space-time yield 6.07 g/(g) cat ·h)。
Example 2:
the catalyst B1 of this example is: the mass fraction of Ru is 2.1%, the active component is ruthenium oxychloride, and the carrier is 80% rutile TiO 2 And 20% anatase TiO 2 (ii) a Fresh catalyst realizes Cl 2 Space-time yield 6.36 g/(g) cat H) Cl after 500h 2 The space-time yield drops to 2.06 g/(g) cat ·h)；
The reaction gas circuit is closed and CH is introduced 3 I and N 2 Mixed gas (H) of 2 The volume fraction is 40 percent, and the rest is N 2 ) The flow rate is 200ml/min, the heating temperature is 320 ℃, and the heating time is kept for 1.5h; then close H 2 Gas path, holding N 2 Displacing for 10min, heating to 360 deg.C, introducing 10ml/min of O 2 And keeping for 3.0h to obtain a regenerated catalyst B2;
b2 was reevaluated according to the same reaction conditions as described above, and the initial activity reached Cl 2 Space-time yield 5.88 g/(g) cat ·h)。
Example 3:
catalyst C1 of this example is: the mass fraction of Ru is 2.6%, the active component is ruthenium oxide, 1.4% of Si is added as a structural auxiliary agent, and the carrier is 75% of rutile TiO 2 And 25% anatase TiO 2 (ii) a Fresh catalyst realizes Cl 2 Space-time yield 6.52 g/(g) cat H) Cl after 500h 2 The space-time yield drops to 4.37 g/(g) cat ·h)；
The reaction gas circuit is closed and H is introduced 2 And N 2 Mixed gas (H) of 2 The volume fraction is 50 percent, and the rest is N 2 ) The flow rate is 100ml/min, the heating temperature is 320 ℃, and the heating time is kept for 3.0h; then close H 2 Gas path, holding N 2 Displacing for 10min, heating to 380 deg.C, introducing 10ml/min of O 2 And keeping for 2.5h to obtain a regenerated catalyst C2;
the C2 was reevaluated according to the same reaction conditions as described above, and the initial activity reached Cl 2 Space-time yield 6.32 g/(g) cat ·h)。
Example 4:
catalyst A2 was evaluated continuously and after 500h of reaction Cl 2 The space-time yield drops to 2.77 g/(g) cat H); catalyst A3 was obtained after regeneration in accordance with the regeneration method of example 1 and evaluated to reach Cl in the initial activity 2 Space-time yield 6.01 g/(g) cat ·h)。
Example 5:
catalyst B2 was evaluated continuously and after 500h of reaction Cl 2 The space-time yield decreased to 1.96 g/(g) cat H); catalyst B3 was obtained after regeneration in accordance with the regeneration method of example 2, and the initial activity after evaluation reached Cl 2 Space-time yield 5.86 g/(g) cat ·h)。
Example 6:
catalyst C2 was evaluated continuously and after 500h of reaction Cl 2 The space-time yield drops to 4.00 g/(g) cat H); catalyst C3 was obtained after regeneration according to the regeneration method of example 3, and the initial activity after evaluation reached Cl 2 Space-time yield 6.28 g/(g) cat ·h)。
Regeneration Performance (Cl) of the regenerated catalyst of each of the above examples 2 Space-time yield, unit: g/(g) cat H)) are shown in table 1 below. The performance of the regenerated catalyst is basically equivalent to that of a fresh catalyst, and the regenerated catalyst can be regenerated and recycled for multiple times, and the regeneration activity is kept at a higher level.
TABLE 1
The initial activity column in table 1 is the activity of catalysts A1, B1, C1 in sequence; the first regeneration activity column is the activity of the catalysts A2, B2 and C2 in sequence; the second regeneration activity is the activity of catalysts A3, B3, C3 in that order.
Claims (10)
1. A method for regenerating a catalyst having ruthenium as an active component and supported on a carrier, comprising:
(1) Treating the catalyst in a mixed atmosphere of reducing gas and inert gas at 100-700 ℃; the reducing gas is H 2 、CH 3 I、CH 2 I 2 And CH 4 One or more of the following;
(2) Roasting the catalyst treated in the step (1) under the conditions of mixed gas flow of oxygen and inert gas and 100-700 ℃.
2. The process for regenerating a hydrogen chloride oxidation catalyst according to claim 1, wherein the regeneration process is carried out in situ in a reactor for the catalytic oxidation of hydrogen chloride.
3. The method for regenerating a hydrogen chloride oxidation catalyst according to claim 1, wherein the active component is ruthenium oxide or ruthenium oxychloride.
4. The process for regenerating a hydrogen chloride oxidation catalyst according to claim 1, wherein the support is rutile titanium dioxide or anatase titanium dioxide or a mixture of both.
5. The method for regenerating a hydrogen chloride oxidation catalyst according to claim 4, wherein the mass fraction of anatase titanium dioxide in the mixture is 10% to 60%.
6. The method for regenerating a hydrogen chloride oxidation catalyst according to claim 1, wherein the step (1) is carried out at 200 to 500 ℃ and the step (2) is carried out at 200 to 400 ℃ for calcination.
7. The method for regenerating a hydrogen chloride oxidation catalyst according to claim 1, wherein the mixed gas of the reducing gas and the inert gas contains the reducing gas in an amount of 20 to 100% by volume.
8. The method for regenerating a hydrogen chloride oxidation catalyst according to claim 1, wherein the mixed gas of oxygen and an inert gas contains 5 to 100% by volume of oxygen.
9. The method for regenerating a hydrogen chloride oxidation catalyst according to claim 1, wherein the inert gas is nitrogen, helium or argon.
10. A method for preparing chlorine through catalytic oxidation of hydrogen chloride, which is characterized in that in the process of preparing chlorine through catalytic oxidation of hydrogen chloride, a catalyst with reduced activity is not removed from a reactor, and the catalyst is directly subjected to in-situ regeneration in the reactor by the method in claim 1, and then the chlorine is continuously prepared.
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Citations (10)
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|---|---|---|---|---|
| CN1154340A (en) * | 1995-09-12 | 1997-07-16 | 巴斯福股份公司 | Preparation of chlorine from hydrogen chloride |
| CN101331240A (en) * | 2005-12-23 | 2008-12-24 | 巴斯夫欧洲公司 | Method for the recovery of ruthenium from used ruthenium oxide-containing catalysts |
| US20090023822A1 (en) * | 2007-07-19 | 2009-01-22 | Tijm Peter J | Method for activating and regenerating catalyst for a fischer-tropsch synthesis reaction |
| CN102271807A (en) * | 2008-12-30 | 2011-12-07 | 巴斯夫欧洲公司 | Method for regenerating a catalyst containing ruthenium oxide for hydrogen chloride oxidation |
| CN102333589A (en) * | 2009-02-26 | 2012-01-25 | 巴斯夫欧洲公司 | Catalyst for hydrogen chloride oxidation comprising ruthenium and silver and/or calcium |
| CN102803130A (en) * | 2009-06-10 | 2012-11-28 | 巴斯夫欧洲公司 | Method for hydrogen chloride oxidation at a catalyst having low surface roughness |
| CN103285882A (en) * | 2012-02-27 | 2013-09-11 | 清华大学 | Regenerating method of deactivated catalyst |
| CN110621403A (en) * | 2017-05-19 | 2019-12-27 | 科思创德国股份有限公司 | Process for regenerating poisoned catalyst containing ruthenium or ruthenium compounds |
| CN113145149A (en) * | 2020-01-07 | 2021-07-23 | 中国科学院大连化学物理研究所 | Regeneration method and application of nitrogen-containing carbon catalyst |
| CN113275020A (en) * | 2020-02-19 | 2021-08-20 | 万华化学（宁波）有限公司 | Regeneration method of catalyst for preparing chlorine by oxidizing hydrogen chloride |
-
2022
- 2022-06-24 CN CN202210728328.XA patent/CN115155672A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1154340A (en) * | 1995-09-12 | 1997-07-16 | 巴斯福股份公司 | Preparation of chlorine from hydrogen chloride |
| CN101331240A (en) * | 2005-12-23 | 2008-12-24 | 巴斯夫欧洲公司 | Method for the recovery of ruthenium from used ruthenium oxide-containing catalysts |
| US20090023822A1 (en) * | 2007-07-19 | 2009-01-22 | Tijm Peter J | Method for activating and regenerating catalyst for a fischer-tropsch synthesis reaction |
| CN102271807A (en) * | 2008-12-30 | 2011-12-07 | 巴斯夫欧洲公司 | Method for regenerating a catalyst containing ruthenium oxide for hydrogen chloride oxidation |
| CN102333589A (en) * | 2009-02-26 | 2012-01-25 | 巴斯夫欧洲公司 | Catalyst for hydrogen chloride oxidation comprising ruthenium and silver and/or calcium |
| CN102803130A (en) * | 2009-06-10 | 2012-11-28 | 巴斯夫欧洲公司 | Method for hydrogen chloride oxidation at a catalyst having low surface roughness |
| CN103285882A (en) * | 2012-02-27 | 2013-09-11 | 清华大学 | Regenerating method of deactivated catalyst |
| CN110621403A (en) * | 2017-05-19 | 2019-12-27 | 科思创德国股份有限公司 | Process for regenerating poisoned catalyst containing ruthenium or ruthenium compounds |
| CN113145149A (en) * | 2020-01-07 | 2021-07-23 | 中国科学院大连化学物理研究所 | Regeneration method and application of nitrogen-containing carbon catalyst |
| CN113275020A (en) * | 2020-02-19 | 2021-08-20 | 万华化学（宁波）有限公司 | Regeneration method of catalyst for preparing chlorine by oxidizing hydrogen chloride |
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