CN103894219A - Fluorination catalyst regeneration method - Google Patents
Fluorination catalyst regeneration method Download PDFInfo
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- Y02P20/584—Recycling of catalysts
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Abstract
The invention relates to a fluorination catalyst regeneration method which comprises a high-temperature purging process, a high-temperature regenerating process, a ratio of transformation generating process and a high-pressure generating process, wherein the high-temperature purging process is that a high-temperature catalyst is purged through high-temperature nitrogen; the high-temperature regenerating process is that the catalyst is regenerated through a mixed gas containing less gas capable of reacting with carbon; the ratio of transformation generating process is that the content of reaction gas in the mixed gas is constantly increased to regenerate the catalyst; the high-pressure generating process is that the mixed gas regenerates the catalyst under the condition that the environment stress of a regeneration system is constantly increased. The method can enable the activity of the catalyst to recover to initial activity.
Description
Technical field
The present invention relates to the renovation process for fluoric ether preparation technology's fluorination catalyst.
Background technology
HFA 134a (HFC-134a) and pentafluoroethane (HFC-125) belong to ODS(ODS) substitute, belong to environmental protection novel refrigerant.HFA 134a (HFC-134a) and pentafluoroethane (HFC-125) can, by HF and alkenyl halide under catalysis of solid catalyst effect, react and make under the condition of certain temperature, pressure and time of contact.Chinese invention patent ZL01141970.9 discloses a kind of fluorination catalyst prepared by HFA 134a that can be used for, and this fluorination catalyst structural formula is CrX
0.005-0.5y
0.005-0.3o
0.1-1.0f
1.0-3.0, wherein X is Mn, Co or Zn, Y is Mg or Ni.This catalyst has active high, good stability, the advantages such as long service life.But because of the reason such as alkane, chloralkane compounds high temperature cabonization generating after alkenyl halide or reaction, this catalyst in use for some time catalytic efficiency reduces even inactivation.The conventional regeneration method of metallic catalyst is that catalyst is contacted to certain hour at a certain temperature with such as air or oxygen of regeneration gas etc.This renovation process is better for the regeneration effect of most metals catalyst, but for having the fluorination catalyst of described structure, regeneration effect is unsatisfactory, and the activity of the catalyst after regeneration only can reach 50%～60% of fresh catalyst.In addition, also exist make fluorination catalyst specific area on the low side and cause the catalytic activity decay of catalyst fast, the problem such as target product selectivity is low.Therefore, be necessary to provide a kind of renovation process that is suitable for above-mentioned fluorination catalyst.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of renovation process of fluorination catalyst.
For solving above technical problem, the present invention takes following technical scheme:
A renovation process for fluorination catalyst, the structural formula of described fluorination catalyst is CrX
0.005-0.5y
0.005-0.3o
0.1-1.0f
1.0-3.0, wherein X is Mn, Co or Zn, and Y is Mg or Ni, and described renovation process comprises the steps:
(1) high-temperature blowing operation: fluorination catalyst is added in fixed bed reactors, be heated to 250～400 ℃, the nitrogen that continues to pass into pressure and be 0.1～0.9MPa, temperature and be 250～400 ℃ purges fluorination catalyst, and be 0.01 second to 1 hour the time of contact of wherein controlling nitrogen and catalyst;
(2) high temperature regeneration operation: complete after high-temperature blowing operation, continue to pass into temperature and be first regeneration gas of 250～400 ℃ under normal pressure, this first regeneration gas contains nitrogen and is selected from O
2, O
3, N
2at least one in O, wherein O
2, O
3, N
2the volume ratio sum of O is 2%～12%, and be 0.01 second to 1 hour the time of contact of controlling the first regeneration gas and fluorination catalyst;
(3) no-load voltage ratio step for regeneration: controlling fluorination catalyst temperature is 250～400 ℃, continues to pass into temperature and is second regeneration gas of 250～400 ℃ under normal pressure, the second regeneration gas contains nitrogen and is selected from O
2, O
3, N
2at least one in O, be 0.01 second to 1 hour the time of contact of controlling the second regeneration gas and fluorination catalyst, O in described the second regeneration gas
2, O
3, N
2o volume ratio sum progressively increases with the increase that passes into the time, O in the second regeneration gas that starts to pass into most
2, O
3, N
2o volume ratio sum is 2%～12%, O in the second regeneration gas finally passing into
2, O
3, N
2o volume ratio sum is 5%～25%;
(4) high-pressure regeneration operation: controlling fluorination catalyst temperature is 250～400 ℃, continues to pass into temperature and is the 3rd regeneration gas of 250～400 ℃, O in the 3rd regeneration gas
2, O
3, N
2o volume ratio sum is 2%～25%, be 0.01 second to 1 hour the time of contact of controlling the 3rd regeneration gas and fluorination catalyst, initial pressure in fixed bed reactors is normal pressure, and the increase that passes into the time with the 3rd regeneration gas progressively rises to 0.15～0.5MPa, then maintains more than 20 hours.
Preferably, in step (1), be 15～40 minutes the time of contact of controlling nitrogen and catalyst.
Preferably, described the first regeneration gas is mixed by nitrogen and air or oxygen,
Preferably, in step (2), be 15～40 minutes the time of contact of controlling the first regeneration gas and fluorination catalyst.
Preferably, in step (3), described the second regeneration gas is mixed by nitrogen and air or oxygen.
Preferably, in step (3), passing in the process of the second regeneration gas, the temperature of fluorination catalyst is tested, control O in described the second regeneration gas
2, O
3, N
2gathering way of O volume ratio sum, guarantees that the fluctuation of the temperature of fluorination catalyst is no more than 10 ℃.
According to the present invention, step (3) and step (4) are carried out afterwards in step (2), between step (3) and step (4), after an elder generation one, carry out or carry out simultaneously.
Preferably, step (3) step (2) afterwards, step (4) carries out before.
Preferably, in step (3), O in the second regeneration gas that starts to pass into most
2, O
3, N
2o volume ratio sum is 5%～10%, O in the second regeneration gas finally passing into
2, O
3, N
2o volume ratio sum is 15%～25%.
Preferably, in step (4), O in described the 3rd regeneration gas
2, O
3, N
2o volume ratio sum is 15%～25%.
Preferably, in step (4), the 3rd regeneration gas is mixed by nitrogen and air or oxygen.
Preferably, in step (4), the pressure in fixed bed reactors progressively rises to 0.2～0.4MPa from normal pressure.
Due to the enforcement of above technical scheme, the present invention compared with prior art tool has the following advantages:
Adopt the inventive method can successfully realize the regeneration of fluorination catalyst, fluorination catalyst after regeneration is the active level that can return to fresh catalyst not only, and prevent sintering phenomenon appearance in catalyst activation process, increasing specific surface area and pore volume greatly, thereby catalyst activity is high, good stability, other character all obtain fine maintenance as mechanical performance.
The specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described in detail, but the present invention is not limited to following examples.The implementation condition adopting in embodiment can require to do further adjustment according to the difference of concrete use, and not marked implementation condition is the condition in normal experiment.
The old fluorination catalyst using in following examples is prepare and be used in the fluorination catalyst of producing after 134a a period of time according to ZL01141970.9 method, and its structural formula is CrMn
0.3mg
0.1o
0.5f
2.0.
Embodiment 1
Pack quantitative old fluorination catalyst into fixed bed reactors, then carry out as follows successively the regeneration of catalyst:
(1) high-temperature blowing operation: fluorination catalyst is heated to 300 ℃, the nitrogen that continues to pass into pressure and be 0.5MPa, temperature and be 300 ℃ purges fluorination catalyst, be 0.5 hour the time of contact of wherein controlling nitrogen and catalyst, and duration of ventilation is 30 hours;
(2) high temperature regeneration operation: complete after high-temperature blowing operation, under normal pressure, continue to pass into temperature and be first regeneration gas of 300 ℃, this first regeneration gas by nitrogen and air in mass ratio 1:1 mix, 1 hour time of contact controlling the first regeneration gas and fluorination catalyst, duration of ventilation is 40 hours;
(3) no-load voltage ratio step for regeneration: controlling fluorination catalyst temperature is 300 ℃, under normal pressure, continue to pass into temperature and be second regeneration gas of 300 ℃, be 1 hour the time of contact of controlling the second regeneration gas and catalyst, the second regeneration gas is mixed by nitrogen and air, and progressively change the mixed proportion of the two, in the second regeneration gas that most starts to pass into, the ratio of nitrogen and air is 1:1, progressively improve the ratio of air, be extremely finally all air, in this process, temperature to catalyst detects, control gathering way of AIR Proportional, the temperature fluctuation that guarantees catalyst is no more than 10 ℃,
(4) high-pressure regeneration operation: controlling fluorination catalyst temperature is 300 ℃, continue to pass into temperature and be the 3rd regeneration gas of 300 ℃, the 3rd regeneration gas is all air, be 1 hour the time of contact of controlling the 3rd regeneration gas and fluorination catalyst, initial pressure in fixed bed reactors is normal pressure, the increase that passes into the time with the 3rd regeneration gas progressively rises to 0.4MPa, maintains 20 hours, completes the regeneration of fluorination catalyst.
Embodiment 2
Pack quantitative old fluorination catalyst into fixed bed reactors, then carry out as follows successively the regeneration of catalyst:
(1) high-temperature blowing operation: fluorination catalyst is heated to 300 ℃, the nitrogen that continues to pass into pressure and be 0.1MPa, temperature and be 300 ℃ purges fluorination catalyst, be 0.5 hour the time of contact of wherein controlling nitrogen and catalyst, and duration of ventilation is 30 hours;
(2) high temperature regeneration operation: complete after high-temperature blowing operation, under normal pressure, continue to pass into temperature and be first regeneration gas of 300 ℃, this first regeneration gas by nitrogen and air in mass ratio 1:1 mix, 0.5 hour time of contact controlling the first regeneration gas and fluorination catalyst, duration of ventilation is 20 hours;
(3) no-load voltage ratio step for regeneration: controlling fluorination catalyst temperature is 300 ℃, under normal pressure, continue to pass into temperature and be second regeneration gas of 300 ℃, be 0.5 hour the time of contact of controlling the second regeneration gas and catalyst, the second regeneration gas is formed by nitrogen and oxygen mix, and progressively change the mixed proportion of the two, in the second regeneration gas that most starts to pass into, the ratio of nitrogen and oxygen is 10:1, progressively improve the ratio of oxygen, ratio to last nitrogen and oxygen is 3:1, in this process, temperature to catalyst detects, control gathering way of AIR Proportional, the temperature fluctuation that guarantees catalyst is no more than 10 ℃,
(4) high-pressure regeneration operation: controlling fluorination catalyst temperature is 300 ℃, continue to pass into temperature and be the 3rd regeneration gas of 300 ℃, the 3rd regeneration gas is all air, be 1 hour the time of contact of controlling the 3rd regeneration gas and fluorination catalyst, initial pressure in fixed bed reactors is normal pressure, the increase that passes into the time with the 3rd regeneration gas progressively rises to 0.4MPa, maintains 20 hours, completes the regeneration of fluorination catalyst.
Embodiment 3
Pack quantitative old fluorination catalyst into fixed bed reactors, then carry out as follows successively the regeneration of catalyst:
(1) high-temperature blowing operation: fluorination catalyst is heated to 200 ℃, the nitrogen that continues to pass into pressure and be 0.1MPa, temperature and be 200 ℃ purges fluorination catalyst, be 15 minutes the time of contact of wherein controlling nitrogen and catalyst, and duration of ventilation is 30 hours;
(2) high temperature regeneration operation: complete after high-temperature blowing operation, under normal pressure, continue to pass into temperature and be first regeneration gas of 200 ℃, this first regeneration gas by nitrogen and air in mass ratio 1:1 mix, 15 minutes times of contact controlling the first regeneration gas and fluorination catalyst, duration of ventilation is 10 hours;
(3) no-load voltage ratio step for regeneration: controlling fluorination catalyst temperature is 200 ℃, under normal pressure, continue to pass into temperature and be second regeneration gas of 200 ℃, be 40 minutes the time of contact of controlling the second regeneration gas and catalyst, the second regeneration gas is formed by nitrogen and oxygen mix, and progressively change the mixed proportion of the two, in the second regeneration gas that most starts to pass into, the ratio of nitrogen and oxygen is 10:1, progressively improve the ratio of oxygen, ratio to last nitrogen and oxygen is 3:1, in this process, temperature to catalyst detects, control gathering way of AIR Proportional, the temperature fluctuation that guarantees catalyst is no more than 10 ℃,
(4) high-pressure regeneration operation: controlling fluorination catalyst temperature is 200 ℃, continue to pass into temperature and be the 3rd regeneration gas of 200 ℃, the 3rd regeneration gas is all air, be 0.5 hour the time of contact of controlling the 3rd regeneration gas and fluorination catalyst, initial pressure in fixed bed reactors is normal pressure, the increase that passes into the time with the 3rd regeneration gas progressively rises to 0.3MPa, maintains 20 hours, completes the regeneration of fluorination catalyst.
Embodiment 4
Pack quantitative old fluorination catalyst into fixed bed reactors, then carry out as follows successively the regeneration of catalyst:
(1) high-temperature blowing operation: fluorination catalyst is heated to 300 ℃, the nitrogen that continues to pass into pressure and be 0.5MPa, temperature and be 300 ℃ purges fluorination catalyst, be 0.5 hour the time of contact of wherein controlling nitrogen and catalyst, and duration of ventilation is 30 hours;
(2) high temperature regeneration operation: complete after high-temperature blowing operation, under normal pressure, continue to pass into temperature and be first regeneration gas of 300 ℃, this first regeneration gas by nitrogen and air in mass ratio 1:1 mix, 1 hour time of contact controlling the first regeneration gas and fluorination catalyst, duration of ventilation is 40 hours;
(3) high-pressure regeneration operation: controlling fluorination catalyst temperature is 300 ℃, continue to pass into temperature and be the 3rd regeneration gas of 300 ℃, the 3rd regeneration gas is all air, be 1 hour the time of contact of controlling the 3rd regeneration gas and fluorination catalyst, initial pressure in fixed bed reactors is normal pressure, the increase that passes into the time with the 3rd regeneration gas progressively rises to 0.4MPa, maintains 20 hours;
(4) no-load voltage ratio step for regeneration: controlling fluorination catalyst temperature is 300 ℃, under normal pressure, continue to pass into temperature and be second regeneration gas of 300 ℃, be 1 hour the time of contact of controlling the second regeneration gas and catalyst, the second regeneration gas is mixed by nitrogen and air, and progressively change the mixed proportion of the two, in the second regeneration gas that starts to pass into most, the ratio of nitrogen and air is 1:1, progressively improves the ratio of air, to being all finally air, complete the regeneration of catalyst.
Comparative example 1
According to traditional catalyst renovation process, old catalyst is regenerated, specific as follows:
(1) pack quantitative old fluorination catalyst into fixed bed reactors, be heated to 300 ℃, the nitrogen that continues to pass into pressure and be 0.1MPa, temperature and be 300 ℃ purges fluorination catalyst, and be 0.5 hour the time of contact of wherein controlling nitrogen and catalyst, and duration of ventilation is 30 hours;
(2) under normal pressure, continuing to pass into temperature is the air of 300 ℃, controls 2 hours times of contact of air and fluorination catalyst, and duration of ventilation is 40 hours, completes the regeneration of catalyst.
Fluorination catalyst after above-mentioned regeneration is applied to respectively and prepares HFA 134a (HFC-134a), and in evaluation catalytic reaction, the conversion ratio of alkenyl halide, reaction is selective.
1. application process is as follows:
The fluorination catalyst 50ml getting respectively after above-mentioned regeneration packs in the nickel pipe bed bioreactor of Ф 19x2 of fused salt heating, carries out following two-step reaction:
(1)3HF+CCl
2=CHCl→CF
3CH
2Cl+2HCl
(2)3HF+CF
3CH
2Cl→CF
3CH
2F+HCl
Wherein:
(1) anhydrous hydrogen fluoride (HF) and trichloro-ethylene are the ingredient proportion continuous dosing of 10:1 in molar ratio, and controlling reaction temperature is 280 ± 5 ℃, and volume space velocity is 1320/h;
(2) anhydrous hydrogen fluoride and HCFC-133a are the ingredient proportion continuous dosing of 4.5:1 in molar ratio, and controlling reaction temperature is 350 ± 5 ℃, and volume space velocity is 1320/h.
2. result is referring to table 1.
Table 1
Above the present invention is described in detail; its object is to allow the personage who is familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence that all Spirit Essences according to the present invention are done changes or modifies, and all should be encompassed in protection scope of the present invention.
Claims (10)
1. a renovation process for fluorination catalyst, the structural formula of described fluorination catalyst is CrX
0.005-0.5y
0.005-0.3o
0.1-1.0f
1.0-3.0, wherein X is Mn, Co or Zn, Y is Mg or Ni, it is characterized in that: described renovation process comprises the steps:
(1) high-temperature blowing operation: described fluorination catalyst is added in fixed bed reactors, be heated to 250～400 ℃, the nitrogen that continues to pass into pressure and be 0.1～0.9MPa, temperature and be 250～400 ℃ purges described fluorination catalyst, and be 0.01 second to 1 hour the time of contact of wherein controlling nitrogen and catalyst;
(2) high temperature regeneration operation: complete after high-temperature blowing operation, continue to pass into temperature and be first regeneration gas of 250～400 ℃ under normal pressure, this first regeneration gas contains nitrogen and is selected from O
2, O
3, N
2at least one in O, wherein O
2, O
3, N
2the volume ratio sum of O is 2%～12%, and be 0.01 second to 1 hour the time of contact of controlling the first regeneration gas and fluorination catalyst;
(3) no-load voltage ratio step for regeneration: controlling fluorination catalyst temperature is 250～400 ℃, continues to pass into temperature and is second regeneration gas of 250～400 ℃ under normal pressure, described the second regeneration gas contains nitrogen and is selected from O
2, O
3, N
2at least one in O, be 0.01 second to 1 hour the time of contact of controlling the second regeneration gas and fluorination catalyst, O in described the second regeneration gas
2, O
3, N
2o volume ratio sum progressively increases with the increase that passes into the time, O in the second regeneration gas that starts to pass into most
2, O
3, N
2o volume ratio sum is 2%～12%, O in the second regeneration gas finally passing into
2, O
3, N
2o volume ratio sum is 5%～25%;
(4) high-pressure regeneration operation: controlling fluorination catalyst temperature is 250～400 ℃, continues to pass into temperature and is the 3rd regeneration gas of 250～400 ℃, O in described the 3rd regeneration gas
2, O
3, N
2o volume ratio sum is 2%～25%, be 0.01 second to 1 hour the time of contact of controlling the 3rd regeneration gas and fluorination catalyst, initial pressure in described fixed bed reactors is normal pressure, and the increase that passes into the time with the 3rd regeneration gas progressively rises to 0.15～0.5MPa, then maintains more than 20 hours.
2. the renovation process of fluorination catalyst according to claim 1, is characterized in that: in step (1), be 15～40 minutes the time of contact of controlling nitrogen and catalyst.
3. the renovation process of fluorination catalyst according to claim 1, is characterized in that: in step (2), described the first regeneration gas is mixed by nitrogen and air or oxygen.
4. the renovation process of fluorination catalyst according to claim 1, is characterized in that: in step (2), be 15～40 minutes the time of contact of controlling the first regeneration gas and fluorination catalyst.
5. the renovation process of fluorination catalyst according to claim 1, is characterized in that: in step (3), described the second regeneration gas is mixed by nitrogen and air or oxygen.
6. the renovation process of fluorination catalyst according to claim 1, is characterized in that: in step (3), passing in the process of the second regeneration gas, the temperature of fluorination catalyst is tested, control O in described the second regeneration gas
2, O
3, N
2gathering way of O volume ratio sum, guarantees that the fluctuation of the temperature of fluorination catalyst is no more than 10 ℃.
7. the renovation process of fluorination catalyst according to claim 1, is characterized in that: step (3) and step (4) are carried out afterwards in step (2), between step (3) and step (4), after an elder generation one, carries out or carries out simultaneously.
8. the renovation process of fluorination catalyst according to claim 7, is characterized in that: step (3) step (2) afterwards, step (4) carries out before.
9. according to the renovation process of the fluorination catalyst described in claim 7 or 8, it is characterized in that: in step (3), O in the second regeneration gas that starts to pass into most
2, O
3, N
2o volume ratio sum is 5%～12%, O in the second regeneration gas finally passing into
2, O
3, N
2o volume ratio sum is 15%～25%.
10. the renovation process of fluorination catalyst according to claim 8, is characterized in that: in step (4), and O in described the 3rd regeneration gas
2, O
3, N
2o volume ratio sum is 15%～25%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105457688A (en) * | 2015-12-16 | 2016-04-06 | 七台河宝泰隆圣迈煤化工有限责任公司 | Catalyst regeneration method |
| CN107670701A (en) * | 2017-10-16 | 2018-02-09 | 乳源东阳光氟有限公司 | A kind of renovation process of fluorination catalyst |
| CN107899585A (en) * | 2017-10-27 | 2018-04-13 | 乳源东阳光氟有限公司 | A kind of renovation process of fluorination catalyst |
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|---|---|---|---|---|
| CN1071348A (en) * | 1990-09-14 | 1993-04-28 | 帝国化学工业公司 | The method of regeneration of fluorination catalyst |
| CN1166380A (en) * | 1996-05-06 | 1997-12-03 | 奥西蒙特公司 | Process for regeneration of catalyst based on trivalent chromium compounds |
| US5739070A (en) * | 1994-06-03 | 1998-04-14 | Solvay (Societe Anonyme) | Process for regenerating a fluorination catalyst |
| CN1651144A (en) * | 2004-12-23 | 2005-08-10 | 西安近代化学研究所 | Regeneration method of fluorine catalyst with chromium base |
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2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071348A (en) * | 1990-09-14 | 1993-04-28 | 帝国化学工业公司 | The method of regeneration of fluorination catalyst |
| US5739070A (en) * | 1994-06-03 | 1998-04-14 | Solvay (Societe Anonyme) | Process for regenerating a fluorination catalyst |
| CN1166380A (en) * | 1996-05-06 | 1997-12-03 | 奥西蒙特公司 | Process for regeneration of catalyst based on trivalent chromium compounds |
| CN1651144A (en) * | 2004-12-23 | 2005-08-10 | 西安近代化学研究所 | Regeneration method of fluorine catalyst with chromium base |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105457688A (en) * | 2015-12-16 | 2016-04-06 | 七台河宝泰隆圣迈煤化工有限责任公司 | Catalyst regeneration method |
| CN107670701A (en) * | 2017-10-16 | 2018-02-09 | 乳源东阳光氟有限公司 | A kind of renovation process of fluorination catalyst |
| CN107670701B (en) * | 2017-10-16 | 2018-10-16 | 乳源东阳光氟有限公司 | A kind of regeneration method of fluorination catalyst |
| CN107899585A (en) * | 2017-10-27 | 2018-04-13 | 乳源东阳光氟有限公司 | A kind of renovation process of fluorination catalyst |
| CN107899585B (en) * | 2017-10-27 | 2019-10-18 | 乳源东阳光氟有限公司 | A kind of regeneration method of fluorination catalyst |
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|---|---|
| CN103894219B (en) | 2015-09-30 |
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