CN107497420B - Regeneration method of carbon-containing noble metal catalyst - Google Patents
Regeneration method of carbon-containing noble metal catalyst Download PDFInfo
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- CN107497420B CN107497420B CN201710798766.2A CN201710798766A CN107497420B CN 107497420 B CN107497420 B CN 107497420B CN 201710798766 A CN201710798766 A CN 201710798766A CN 107497420 B CN107497420 B CN 107497420B
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- B01J38/00—Regeneration or reactivation of catalysts, in general
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- B01J38/00—Regeneration or reactivation of catalysts, in general
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Abstract
During the combustion, the oxygen content in the regenerated gas is stepped controlled, carbon deposit in the catalyst is eliminated through stepped combustion, and the catalyst is chloridized and reduced to restore the activity of the catalyst. The method has the advantages of mild and easily controlled conditions and simple and convenient operation, solves the problems of difficult control and difficult process production requirement when the domestic high-carbon-content catalyst enters a catalyst continuous production system designed by UOP, avoids the catalyst inactivation phenomenon caused by hydrothermal method regeneration, has good catalytic performance of the regenerated catalyst, is equivalent to a fresh catalyst, reduces the waste of noble metal catalyst, and reduces the production cost.
Description
Technical Field
The invention belongs to the field of catalyst regeneration, and particularly relates to a regeneration method of a carbon-containing noble metal catalyst.
Background
In the reaction of dehydrogenating single-chain olefin from alkane, the reaction is limited by thermodynamic equilibrium and must be carried out under high-temperature and low-pressure conditions. And the excessive temperature inevitably causes coking on the surface of the catalyst, the mobility of the coked catalyst is reduced, the high carbon content of the catalyst is caused by long-time coalescence, the catalyst is inactivated by the high carbon content catalyst, and the inactivated catalyst is easy to block a catalyst bed layer.
At present, domestic propylene plant made by alkane dehydrogenation is accelerated to build, a device which has been operated for about 2 years has high-carbon content catalysts (the carbon content is more than 15 percent), the high-carbon content catalysts enter a catalyst continuous regeneration system designed by UOP, the control is difficult, the process production requirements are difficult to meet, the continuous regeneration of the high-carbon content catalysts cannot be realized, a large amount of high-carbon catalysts are determined to be scrapped catalysts, the waste of precious metal catalysts is caused, and the great loss is caused to an alkane dehydrogenation device.
At present, the method for regenerating the high-carbon catalyst is generally an ex-situ regeneration method, but in the ex-situ regeneration method, moisture is difficult to avoid, the catalyst is easy to be permanently damaged, and chlorine is not injected, so that the loss of chlorine content is caused.
Chinese patent application CN1589970A discloses a regeneration method of a catalyst for producing alkyl alkenyl arene by dehydrogenation of alkyl arene, in which water vapor and air are introduced, and the catalyst is regenerated by a hydrothermal method, which requires a higher regeneration temperature to completely burn off carbon deposited on the catalyst, but for a platinum-containing alkane dehydrogenation high carbon catalyst, the hydrothermal method can directly cause permanent deactivation of the catalyst, and thus is not suitable for an alkane dehydrogenation catalyst.
The chinese patent application CN101940959A discloses a method for regenerating a low-carbon alkane dehydrogenation catalyst, which comprises the steps of firstly regenerating in a low air environment, burning off carbon deposits on the surface of the catalyst and most of the carbon deposits inside a pore channel, and then further regenerating the catalyst under the condition of mixing water vapor and air, but the regeneration process is easy to deactivate the alkane dehydrogenation catalyst.
The Chinese patent application CN104415798A discloses a catalyst regeneration method and a regenerator, the method adopts a scheme of turbulent bed countercurrent contact coking, realizes that the coking time of a spent catalyst on a fluidized bed is constant, the carbon content of the regenerator is consistent, the activity of the regenerator is unchanged, and catalytic cracking can be carried out, such as a regeneration method of catalysts for preparing olefin from methanol, but the regeneration method of the catalysts with large fluctuation of the carbon content is not described. In the regeneration process of the carbon-containing noble metal catalyst, the burning temperature is increased along with the increase of the carbon content during the coke burning regeneration, which is difficult to control and has higher requirement on regeneration equipment.
Disclosure of Invention
The invention aims to provide a regeneration method of a carbon-containing noble metal catalyst, which can continuously regenerate the noble metal catalyst with high carbon content (the carbon content is more than or equal to 8%) generated in alkane dehydrogenation reaction, has mild and easily controlled conditions and simple and convenient operation, has good activity of the regenerated catalyst, is equivalent to a fresh catalyst, and avoids the catalyst deactivation phenomenon caused by hydrothermal regeneration.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for regenerating a carbonaceous noble metal catalyst, comprising the steps of:
1) carrying out primary coking regeneration on the carbon-containing noble metal catalyst, wherein in the process, the oxygen content in the regeneration gas is controlled in a gradient manner, the oxygen content is increased from 0.3-0.6 vol.% to 1.6-2.0 vol.%, and in the process, the combustion peak temperature is 500-615 ℃; wherein the carbon content in the carbon-containing noble metal catalyst is more than or equal to 8 percent;
2) re-burning the carbon-containing noble metal catalyst subjected to preliminary coking regeneration in the step 1), wherein in the process, the oxygen content in the regenerated gas is controlled in a gradient manner, the oxygen content is increased from 1.0-1.3 vol.% to 2.5-4.0 vol.%, and in the process, the combustion peak temperature is 500-615 ℃, and then drying and cooling are carried out to obtain the catalyst to be activated;
3) carrying out chlorination operation on the catalyst to be activated by instrument wind or nitrogen containing chloride, wherein the moisture content in the instrument wind or nitrogen is 0-1ppm, the moisture content in the chloride is 0-2%, and the chloride content is 0.5-1.5% of the coke-burning regeneration quality;
4) and (3) carrying out hydrogen reduction on the catalyst subjected to chlorination operation, wherein the hydrogen concentration is 1-99.99 vol.%, and the reduction temperature is 400-600 ℃ to obtain the regenerated noble metal catalyst.
Preferably, in step 1), the method for controlling the gradient of the oxygen content in the regeneration gas comprises the following steps: firstly, controlling the oxygen content at 0.3-0.6 vol.%, increasing the oxygen content to 1-1.2 vol.% after the combustion peak temperature is stable, and increasing the oxygen content to 1.5-2% after the combustion peak temperature is stable, so that the combustion peak temperature is 500-615 ℃.
Preferably, in step 2), the method for controlling the gradient of the oxygen content in the regeneration gas comprises the following steps: firstly, the oxygen content is controlled to be 1.0-1.3 vol.%, after the peak temperature is stable, the oxygen content is increased by 1 vol.%, after the peak temperature is constant, the next gradient control is carried out, and the combustion peak temperature is 500-615 ℃.
Preferably, the combustion peak temperature in step 1) and/or step 2) is 580-600 ℃.
Preferably, in the step 1) and the step 2), the regeneration mass of the scorch is 0-800kg/h or 200-400 kg/h.
Preferably, in the step 3), the moisture content in the instrument wind is 0-0.5ppm, the moisture content in the chloride is 0-100ppm, the using amount of the chloride is 0.6-1.0% of the coke-burning regeneration mass, and the chloride is selected from one or a mixture of several of chlorine, hydrogen chloride, carbon tetrachloride or tetrachloroethane
Preferably, in the step 4), the hydrogen concentration is 99.99 vol.%, and the reduction temperature is 530-.
And, the carbon-containing noble metal catalyst is Al2O3The carrier is the noble metal which is platinum.
Further, the carbon content in the carbon-containing noble metal catalyst in step 1) is 8-25 wt.%, preferably 15-25 wt.%.
In the primary coking process and the further combustion process, the oxygen concentration in the regeneration gas is subjected to gradient control, so that the oxygen concentration in the regeneration gas is slowly changed to control the peak temperature of combustion, the peak temperature is controlled to be 500-615 ℃, and equipment is effectively protected.
In the regeneration process of the noble metal catalyst, when the chlorination operation is carried out, if the moisture content is too high, the activity of the catalyst is reduced, so the invention strictly controls the moisture in the process gas and the maximum value of the operation temperature to ensure that equipment is not damaged in the operation process.
Compared with the prior art, the invention has the beneficial effects that:
1) the invention carries out in-tower regeneration on the high carbon-containing catalyst in the alkane dehydrogenation single-chain olefin reaction, controls the change mode of oxygen content in the scorching process, well controls the peak temperature, reduces the factors of equipment damage, reduces the equipment requirement, is simple and convenient to operate, and solves the problems that the existing domestic high carbon-containing catalyst enters the existing catalyst continuous production system, is difficult to control and is difficult to meet the process production requirement.
2) In the invention, the noble metal catalyst is regenerated in the tower, the moisture content is strictly controlled, compared with the regeneration outside the device applied in the prior art, the damage of moisture to the catalyst is avoided, and the activity of the regenerated catalyst is good.
3) The carbon-containing noble metal catalyst can be continuously regenerated by utilizing the method, the selectivity and the activity of the regenerated catalyst are equivalent to those of a fresh catalyst, the waste of the noble metal catalyst is reduced by the regeneration and the recycling of the catalyst, and the production cost is reduced.
Drawings
FIG. 1 shows the selectivity comparison of the regenerated catalyst and the fresh catalyst in examples 1 and 2 of the present invention.
FIG. 2 shows the results of comparing the conversion of the regenerated catalyst with that of the fresh catalyst in examples 1 and 2 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following specific examples, which do not limit the scope of the present invention.
Example 1 cyclic regeneration of a noble metal catalyst having a carbon content of 15 wt.%
In the dehydrogenation reaction of propane, 10 tons of platinum-containing catalyst to be regenerated, the average carbon content of which is 15%, was transferred into a separation hopper through a small catalyst addition hopper under a nitrogen atmosphere.
Carrying out primary coke-burning regeneration on a noble metal catalyst in a hopper, wherein the coke-burning regeneration mass is 300kg/h, and in the process, the oxygen content in the regeneration gas is 0.6-1.3 vol.%, and carrying out gradient control: when the oxygen content is 0.6%, after the combustion peak temperature is stabilized at 575 ℃, the oxygen content is increased to 1%, after the combustion peak temperature is stabilized at 588 ℃, the oxygen content is increased to 1.3%, and the combustion peak temperature is stabilized at 600 ℃.
And (2) burning the carbon-containing noble metal catalyst regenerated by the primary coking again, wherein the oxygen content in the regenerated gas is 1.3-3 vol.%, and performing gradient control: when the oxygen content is 1.3 vol.%, after the combustion peak temperature is stabilized at 570 ℃, the oxygen content is increased to 2 vol.%, after the combustion peak temperature is stabilized at 580 ℃, the oxygen content is increased to 3 vol.%, the combustion peak temperature is stabilized at 610 ℃, and after the combustion is finished, the regenerant to be activated is further dried and cooled.
Then instrument wind or nitrogen gas containing chlorine gas (2.4kg/h) is injected into the regenerant to be activated, and the metal platinum is dispersed again, wherein the moisture content in the instrument wind or the nitrogen gas is 0-1ppm, and the moisture content in the chlorine gas is 0-2%.
After the chlorination operation was completed, the material was transferred to a reduction zone, and 99.99 vol.% hydrogen was introduced for reduction at a reduction temperature of 600 ℃ to obtain 8.5t of regenerated platinum-containing catalyst.
Example 2 cyclic regeneration of a noble metal catalyst with a carbon content of 25 wt.%
In the dehydrogenation reaction of propane, 3 tons of platinum-containing catalyst to be regenerated, the average carbon content of which is 25%, was transferred into a separation hopper through a small catalyst addition hopper under a nitrogen atmosphere.
The method comprises the steps of carrying out primary coking regeneration on a noble metal catalyst in a hopper, wherein the coking regeneration mass is 100kg/h, in the process, the oxygen content in the regeneration gas is 0.5-1.3 vol.%, and carrying out gradient control, the oxygen content is increased in a gradient manner of 0.5 vol.%, 1 vol.%, 1.2 vol.%, and 1.3 vol.%, each gradient is maintained for 1h, and the temperature of a peak value to be combusted is stabilized at 580-.
And (2) burning the carbon-containing noble metal catalyst regenerated by the primary coking again, wherein in the process, the oxygen content in the regenerated gas is 1.3-3%, and gradient control is carried out: when the oxygen content is 1.3 vol.%, after the combustion peak temperature is stabilized at 570 ℃, the oxygen content is increased to 2 vol.%, after the combustion peak temperature is stabilized at 580 ℃, the oxygen content is increased to 3 vol.%, the combustion peak temperature is stabilized at 610 ℃, and after the combustion is finished, the regenerant to be activated is further dried and cooled.
Then, instrument wind/nitrogen gas containing chlorine gas (2.4kg/h) is injected into the regenerant to be activated, and the metal platinum is dispersed again, wherein the moisture content in the instrument wind or the nitrogen gas is 0-1ppm, and the moisture content in the chlorine gas is 0-2%.
After the chlorination operation was completed, the material was transferred to a reduction zone, and 99.99 vol.% hydrogen was introduced for reduction at a reduction temperature of 600 ℃ to obtain 2.26t of regenerated platinum-containing catalyst.
Example 3 Performance testing
The regenerated noble metal catalysts obtained in inventive examples 1 and 2 were tested and compared with fresh catalysts, respectively, for propane dehydrogenation, under experimental conditions: 625 ℃, H/HC 0.5, liquid hourly space velocity 3 ton/ton, see fig. 1-fig. 2.
As can be seen from fig. 1-2, the regenerated catalyst of the present invention has no obvious decrease in catalyst selectivity (fig. 1) and substrate conversion (fig. 2) compared with the fresh catalyst, and the regeneration effect is ideal.
Claims (12)
1. A method for regenerating a carbonaceous noble metal catalyst, comprising the steps of:
1) carrying out primary coking regeneration on the carbon-containing noble metal catalyst, wherein in the primary coking regeneration process, the oxygen content in the regeneration gas is controlled in a gradient manner, the oxygen content is increased from 0.3-0.6 vol.% to 1.6-2.0 vol.%, and in the primary coking regeneration process, the combustion peak temperature is 500-615 ℃; wherein the carbon content in the carbon-containing noble metal catalyst is more than or equal to 15 wt.%;
2) re-burning the carbon-containing noble metal catalyst subjected to preliminary coking regeneration in the step 1), in the re-burning process, controlling the oxygen content in the regenerated gas in a gradient manner, increasing the oxygen content from 1.0-1.3 vol.% to 2.5-4.0 vol.%, in the re-burning process, the burning peak temperature is 500-;
3) carrying out chlorination operation on the catalyst to be activated by instrument wind or nitrogen containing chloride, wherein the moisture content in the instrument wind or nitrogen is 0-1ppm, the moisture content in the chloride is 0-2%, and the using amount of the chloride is 0.5-1.5% of the regeneration quality of the scorch;
4) and (3) carrying out hydrogen reduction on the catalyst subjected to chlorination operation, wherein the hydrogen concentration is 1-99.99 vol.%, and the reduction temperature is 400-600 ℃ to obtain the regenerated noble metal catalyst.
2. The method for regenerating a carbon-containing noble metal catalyst according to claim 1, wherein the gradient control method of the oxygen content in the regeneration gas in step 1) is: firstly, controlling the oxygen content at 0.3-0.6 vol.%, increasing the oxygen content to 1-1.2 vol.% after the combustion peak temperature is stabilized, and increasing the oxygen content to 1.6-2 vol.% after the combustion peak temperature is stabilized, wherein the combustion peak temperature is stabilized at 500-.
3. The method for regenerating a carbon-containing noble metal catalyst according to claim 1, wherein the gradient control method of the oxygen content in the regeneration gas in the step 2) is: firstly, controlling the oxygen content at 1.0-1.3 vol.%, increasing the oxygen content by 1% gradient after the peak temperature is stable, and controlling the next gradient after the peak temperature is constant, wherein the combustion peak temperature is controlled to be 500-615 ℃.
4. The method for regenerating a carbon-containing noble metal catalyst as claimed in any one of claims 1 to 3, wherein the combustion peak temperature in step 1) and/or step 2) is 580-600 ℃.
5. The method for regenerating a carbon-containing noble metal catalyst according to claim 1, wherein in the step 3), the coke-burning regeneration mass is 0 to 800 kg/h.
6. The method for regenerating a carbon-containing noble metal catalyst as claimed in claim 1, wherein the coke-burning regeneration mass in step 3) is 200-400 kg/h.
7. The method for regenerating a carbonaceous noble metal catalyst as claimed in claim 1, wherein the moisture content in the meter air in step 3) is 0 to 0.5ppm, and the moisture content in the chloride is 0 to 100 ppm.
8. The method for regenerating a carbon-containing noble metal catalyst according to claim 7, wherein the amount of the chloride used in step 3) is 0.6 to 1.0% by mass based on the regenerated mass of the char, and the chloride is selected from one or a mixture of chlorine, hydrogen chloride, carbon tetrachloride and tetrachloroethane.
9. The method as claimed in claim 1, wherein the hydrogen concentration in step 4) is 99.99 vol.%, and the reduction temperature is 530 ℃ and 560 ℃.
10. The method for regenerating a carbon-containing noble metal catalyst according to claim 1, wherein the carbon-containing noble metal catalyst is Al2O3The carrier is the noble metal which is platinum.
11. The method for regenerating a carbon-containing noble metal catalyst according to any one of claims 1 to 3 or 5 to 10, characterized in that the carbon content in the carbon-containing noble metal catalyst in step 1) is 15 to 25 wt.%.
12. The method for regenerating a carbon-containing noble metal catalyst according to claim 4, wherein the carbon content in the carbon-containing noble metal catalyst in step 1) is 15 to 25 wt.%.
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| US7771977B2 (en) * | 2006-09-29 | 2010-08-10 | National University Corporation NARA Institute of Science and Technology | Alkane polyol dehydrogenase |
| CN104084218A (en) * | 2014-07-10 | 2014-10-08 | 南京沃来德能源科技有限公司 | Method for regenerating light alkane dehydrogenation catalyst |
| CN104107704A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | Method for regenerating platinum-containing low carbon alkane dehydrogenation catalyst |
| CN106391138A (en) * | 2016-08-31 | 2017-02-15 | 中国科学院福建物质结构研究所 | In-situ regeneration method of Pd catalyst for CO dehydrogenation purification |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7771977B2 (en) * | 2006-09-29 | 2010-08-10 | National University Corporation NARA Institute of Science and Technology | Alkane polyol dehydrogenase |
| CN101722012A (en) * | 2008-10-15 | 2010-06-09 | 赢创德固赛有限责任公司 | Moulding activated metal fixed bed catalyst |
| CN104107704A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | Method for regenerating platinum-containing low carbon alkane dehydrogenation catalyst |
| CN104084218A (en) * | 2014-07-10 | 2014-10-08 | 南京沃来德能源科技有限公司 | Method for regenerating light alkane dehydrogenation catalyst |
| CN106391138A (en) * | 2016-08-31 | 2017-02-15 | 中国科学院福建物质结构研究所 | In-situ regeneration method of Pd catalyst for CO dehydrogenation purification |
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