CN104475175A - Method for generating palladium catalyst for producing hydrogen peroxide by using anthraquinone process - Google Patents
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Abstract
The invention discloses a method for generating a palladium catalyst for producing hydrogen peroxide by using an anthraquinone process. The method comprises the following comprehensive regeneration steps: soaking or circularly washing a catalyst to be regenerated by using aromatic hydrocarbon with temperature of 30-70 DEG C, treating by using saturated steam with temperature of 100-120 DEG C, soaking or circularly washing by using hot water with temperature of 30-95 DEG C, displacing with nitrogen, activating with nitrogen, and the like. The regenerated catalyst is thorough in regeneration degree, good in activity recovery, and long in regeneration period and service life.
Description
Technical field:
The present invention relates to a kind of regeneration treating method of palladium catalyst of hydrogen dioxide solution production by anthraquinone process, belong to catalyst optimization operation technique.
Background technology:
Hydrogen peroxide (H
2o
2) be a kind of important chemical products, be widely used in the fields such as papermaking, weaving, chemicals synthesis, military project, electronics, food processing, medicine, environmental protection, metallurgy.H
2o
2production method mainly comprise electrolysis, anthraquinone, isopropanol method and hydrogen-oxygen direct synthesis technique etc., wherein anthraquinone is the most frequently used production method, at present at home and abroad equal dominate.
Anthraquinone employing anthraquinone is worked carrier, finally obtains H by hydrogenation, oxidation, extraction three main process
2o
2, wherein anthraquinone hydrogenation generates the reaction of hydrogen anthraquinone is one of committed step.Anthraquinone hydrogenation reaction belongs to gas-liquid-solid three phase catalytic reaction, and be in static or motion state according to catalyst and be divided into again fixed bed reactors and the large class of fluidized-bed reactor two, domestic most device adopts fixed bed reactors.
Anthraquinone fixed bed hydrogenation is produced in hydrogen peroxide process, anthraquinone hydrogenation with palladium catalyst in use for some time, surface slowly can by some anthraquinone degradation products, alumina powder and raw material with a small amount of impurity institute coated, the contact surface of active substance palladium and working solution and hydrogen in catalyst will be reduced so gradually, cause catalyst activity more and more lower, when catalyst hydrogenation performance can not meet production requirement, catalyst just needs regeneration.The renovation process that current palladium catalyst is conventional is steam treatment method and organic solvent infusion method.Namely steam treatment method is blown into a large amount of steam in beds, the organic matter of catalyst surface and most inorganic salts are attached to by vapours washing, the capped activated centre of catalyst surface is exposed again, thus recovery catalyst activity, this processing method is better for catalyst top bed regeneration effect, along with steam deeply and the stop of catalyst and cooling, enter a steam slowly to become hot water and cause flow sharply to reduce, flow out from the short circuit of lower catalyst bed layer, Lower Half major part catalyst is caused to regenerate, overall regeneration effect is not good.Organic solvent infusion method many employings heavy aromatics, trioctyl phosphate or the mixed solvent of the two soak catalyst, with the anthraquinone system organic matter that catalyst-solvent surface attaches, but this processing method is little to inorganic salts removal effects such as oxygen aluminium powders, and overall regeneration effect is also undesirable.
Summary of the invention:
The object of the invention is to overcome the deficiency of above-mentioned prior art and provides a kind of renovation process of palladium catalyst of hydrogen dioxide solution production by anthraquinone process, and it is thorough that the method has catalyst regeneration, and activation recovering is good, can extending catalyst regeneration period and service life.
Object of the present invention can be reached by following measure: a kind of renovation process of palladium catalyst of hydrogen dioxide solution production by anthraquinone process, it is characterized in that it comprises the steps:
A) will the catalyst of regeneration be needed to soak 8-16 hour with the aromatic hydrocarbons of 30-70 DEG C in device or pass through circulating pump circulation flushing 8-16 hour with the aromatic hydrocarbons of 30-70 DEG C; Aromatic hydrocarbons addition is as the criterion with complete submergence catalyst;
B) catalyst is with the saturated steam process 16-48h of 100-120 DEG C in device, and wherein steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, as clear as crystal for terminal with steam condensate (SC);
C) catalyst passes through circulating pump circulation flushing 8-24h with 30-95 DEG C of hot-water soak 8-24h or with 30-95 DEG C of hot water in device, soak or every half an hour, hot water sampled in circulation flushing process, after water muddiness is dirty, addle is discharged and again fill into 30-95 DEG C of hot water continuation immersion or circulation flushing, as clear as crystal for terminal with sampling water;
D) catalyst after above-mentioned immersion or circulation flushing carries out nitrogen displacement, Hydrogen activation process, and within activation temperature controls room temperature ~ 80 DEG C, catalyst activation is complete can come into operation again.
In order to realize object of the present invention further, by after the catalyst emptying hot water after immersion or circulation flushing in described step d), pass into 100-150 DEG C of hot nitrogen catalyst is dried up, catalyst dries up rear maintenance positive pressure of nitrogen atmosphere and slowly passes into hydrogen and carry out activation process to catalyst, within activation temperature controls room temperature ~ 80 DEG C, catalyst activation is complete can come into operation again.
In order to realize object of the present invention further, by after the catalyst emptying hot water after immersion or circulation flushing in described step d), cooling catalyst is drawn off to 30-40 DEG C from fixed bed, wash after soaking half an hour with 20-50 DEG C of aromatic hydrocarbons, be washed till catalyst surface bright and clean without till organic addendum, catalyst is put into the dry aromatic hydrocarbons in stainless steel mesh overhead afterwards, by the catalyst 30-50 of dry for sky aromatic hydrocarbons DEG C of deionized water washing, after washes clean, catalyst taking-up is put into the empty solid carbon dioxide of stainless steel mesh and divides; Afterwards catalyst is dried, dry packaging after sieving to put well, after whole catalyst treatment, catalyst is backfilling into hydrogenation tower again, the qualified rear nitrogen of hydrogenation tower leak test is replaced, slowly Hydrogen activation is passed into after nitrogen displacement is qualified, within activation temperature controls room temperature-80 DEG C, catalyst activation is complete can come into operation again.
In order to realize object of the present invention further, described will to soak or after catalyst emptying hot water after circulation flushing, then use 60 DEG C, 30 DEG C deionized water circular treatment twice respectively, fixed bed temperature is down to 30-40 DEG C, then water is put only; The catalyst cooling the temperature to 30-40 DEG C draws off from fixed bed.
In order to realize object of the present invention further, in described step c), hot water temperature is 80-95 DEG C.
The present invention can produce following good effect compared with the prior art: the inventive method adopts aromatic hydrocarbons, steam, hot water to carry out integrated treatment catalyst, first soak with aromatic hydrocarbons or circulation dissolving anthraquinone system organic matter, use steam treatment catalyst again, finally add a large amount of hot water hydride circulating pump circulation cleaning catalyst, because hot water flow is very large, at utmost can eliminate the Effect of Short Circuit of steam treatment, remove the impurity such as the oxygen aluminium powder causing the anthraquinone system organic matter of catalysqt deactivation and surface to attach more thoroughly.May have the fixed bed of caking for the low and bed inner catalyst of operating condition difference catalyst activity, catalyst can be clawed after above-mentioned process, reusable heat aromatic hydrocarbons and the thorough cleaning catalyst of hot water, dry backfill afterwards, again come into operation after Hydrogen activation.
Detailed description of the invention: below the specific embodiment of the present invention is elaborated:
If control better without extraction band scale tower band alkali phenomenon in plant running process, system anthraquinone less working solution of degrading is cleaner, the carclazyte that carclazyte bed more swaps out is without efflorescence, hydrogenation tower catalyst bed layer resistance slowly rises with extending service time, catalyst is without obvious caking phenomenon, can adopt following regeneration treating method, it comprises the steps:
A) catalyst needing in device to regenerate first is soaked 8-16h with the aromatic hydrocarbons of 30-70 DEG C or with the aromatic hydrocarbons of 30-70 DEG C with hydride gas-liquid separator for buffer container hydride circulating pump circular treatment 8-16h, the new working solution of the recyclable preparation of aromatic hydrocarbons after use or directly fill into system; Aromatic hydrocarbons addition is as the criterion with complete submergence catalyst;
B) with the saturated steam process 16-48h of 100-120 DEG C, till steam-condensation water outlet is as clear as crystal, wherein steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, reenters system use in initial stage steam condensate (SC) containing some work liquid is recyclable after alkali cleaning washing process;
C) with 30-95 DEG C of hot-water soak catalyst 8-24 hour or with 30-95 DEG C of hot water with hydride gas-liquid separator for buffer container hydride circulating pump circulation flushing catalyst 8-24 hour, hydride pump flow can reach maximum.Soak or every half an hour, hot water sampled in circulation flushing process, after water muddiness is dirty, addle being discharged and again fill into 30-95 DEG C of hot water continuation immersion or circulation flushing, as clear as crystal for terminal with sampling water;
D) by after the catalyst emptying hot water after immersion or circulation flushing, pass into 100-150 DEG C of hot nitrogen and catalyst is dried up; Catalyst dries up rear maintenance positive pressure of nitrogen atmosphere and slowly passes into hydrogen and carry out activation process to catalyst, and activation temperature controls in room temperature ~ 80 DEG C; Catalyst activation is complete can come into operation again.
If control poorly have extraction band water or washing tower (for removing CO2) band alkali phenomenon in plant running process, system anthraquinone violent working solution of degrading is messy, the carclazyte that carclazyte bed more swaps out has efflorescence, the hydrogenation tower catalyst bed layer resistance short time rises obviously, suspect that catalyst has caking phenomenon, following regeneration treating method, it comprises the steps:
A) catalyst needing in device to regenerate first is soaked 8-16h with the aromatic hydrocarbons of 30-70 DEG C or with the aromatic hydrocarbons of 30-70 DEG C with hydride gas-liquid separator for buffer container hydride circulating pump circular treatment 8-16h, the new working solution of the recyclable preparation of aromatic hydrocarbons after use or directly fill into system; Aromatic hydrocarbons addition is as the criterion with complete submergence catalyst;
B) with the saturated steam process 16-48h of 100-120 DEG C, till steam-condensation water outlet is as clear as crystal, wherein steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, reenters system use in initial stage steam condensate (SC) containing some work liquid is recyclable after alkali cleaning washing process;
C) with 30-95 DEG C of hot-water soak catalyst 8-24 hour or with 30-95 DEG C of hot water with hydride gas-liquid separator for buffer container hydride circulating pump circulation flushing catalyst 8-24 hour, hydride pump flow can reach maximum.Soak or every half an hour, hot water sampled in circulation flushing process, after water muddiness is dirty, addle being discharged and again fill into 30-95 DEG C of hot water continuation immersion or circulation flushing, as clear as crystal for terminal with sampling water;
D) by after the catalyst emptying hot water after immersion or circulation flushing, then use 60 DEG C, 30 DEG C deionized water circular treatment twice respectively, fixed bed temperature is down to 30-40 DEG C, then water is put only; The catalyst cooling the temperature to 30-40 DEG C draws off from fixed bed, wash after soaking half an hour with 20-50 DEG C of aromatic hydrocarbons, period, available wooden rake stirred, catalyst if any caking need by cake broke, be washed till catalyst surface bright and clean without till organic addendum, catalyst is put into the dry aromatic hydrocarbons in stainless steel mesh overhead afterwards, with after the new working solution of the recyclable preparation of aromatic hydrocarbons or directly fill into system; By the catalyst 30-50 of dry for sky aromatic hydrocarbons DEG C of deionized water washing, after washes clean, catalyst taking-up is put into the empty solid carbon dioxide of stainless steel mesh and divides; The catalyst that empty solid carbon dioxide divides is shakeout airing on clean Polypropylence Sheet, dries loading clean packaging bag (plastic lining film) interior tying after sieving and put well; After whole catalyst treatment, catalyst is backfilling into hydrogenation tower again, the qualified rear nitrogen displacement of hydrogenation tower leak test, slowly passes into Hydrogen activation after nitrogen displacement is qualified, and activation temperature controls within room temperature ~ 80 DEG C; Catalyst activation is complete can come into operation again.
Catalyst activity adopts glass fixed bed to evaluate, the each 10g of loaded catalyst, working solution 410ml, 2-EAQ content 100g/L in working solution, working solution solvent adopts trioctyl phosphate (TOP) and heavy aromatics (Ar), ratio of solvent 1:3, hydrogen flowing quantity 0.5L/min, reaction temperature 50 DEG C, reaction pressure is normal pressure.First set reaction adds 50ml working solution, hydrogen pushes the work forward liquid and catalyst reaction, working solution is released with titration of potassium permanganate hydrogenation efficiency half an hour by reaction, second time adds the new working solution of 40ml to the tenth time at every turn and participates in reaction, reaction is released working solution and is measured hydrogenation efficiency after half an hour, getting second time to the tenth hydrogenation efficiency mean value is the activity value of this catalyst.
Embodiment 1:
Get and need regeneration palladium catalyst 10Kg to load regenerating unit, add the aromatic hydrocarbons heat-insulation soaking 16h of 30L 70 DEG C, then aromatic hydrocarbons is drained recovery; Pass into the saturated steam process 16h-48h of 100-120 DEG C again, as clear as crystal for terminal with steam condensate (SC).Saturated steam steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, reuses in initial stage steam condensate (SC) containing some work liquid is recyclable after alkali cleaning washing process; Add 30L 30 DEG C of hot water again, controlled circulation pump discharge 125L/h soak cycles washing 8-24h, every half an hour, hot water is sampled in circulation flushing process, after water muddiness is dirty, addle is discharged and again fill into 30 DEG C of hot water continuation circulation flushings, as clear as crystal for terminal with sampling water; Emptying hot water passes into 100-150 DEG C of hot nitrogen and is dried up by catalyst; Catalyst dries up rear maintenance positive pressure of nitrogen atmosphere and slowly passes into hydrogen and carry out activation process to catalyst, and within activation temperature controls room temperature ~ 80 DEG C, after activation, sampling is surveyed active, hydrogenation efficiency 7.6g/L.
Embodiment 2
Get and need regenerate palladium catalyst 10Kg loading regenerating unit, add the aromatic hydrocarbons of 30L50 DEG C, controlled circulation pump discharge 125L/h soak cycles washing 16h, then drains recovery by aromatic hydrocarbons; Pass into the saturated steam process 16h-48h of 100-120 DEG C again, as clear as crystal for terminal with steam condensate (SC).Saturated steam steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, reuses in initial stage steam condensate (SC) containing some work liquid is recyclable after alkali cleaning washing process; Add 30L 95 DEG C of hot water again, heat-insulation soaking 8-24h, samples hot water every half an hour in immersion process, addle is discharged and again fill into 90 DEG C of hot water continuation immersions after water muddiness is dirty, as clear as crystal for terminal with sampling water; Emptying hot water passes into 100-150 DEG C of hot nitrogen and is dried up by catalyst; Catalyst dries up rear maintenance positive pressure of nitrogen atmosphere and slowly passes into hydrogen and carry out activation process to catalyst, and within activation temperature controls room temperature ~ 80 DEG C, after activation, sampling is surveyed active, hydrogenation efficiency 7.4g/L.
Embodiment 3
Get and need regenerate palladium catalyst 10Kg loading regenerating unit, add the aromatic hydrocarbons of 30L30 DEG C, controlled circulation pump discharge 125L/h soak cycles washing 12h, then drains recovery by aromatic hydrocarbons; Pass into the saturated steam process 16h-48h of 100-120 DEG C again, as clear as crystal for terminal with steam condensate (SC).Saturated steam steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, reuses in initial stage steam condensate (SC) containing some work liquid is recyclable after alkali cleaning washing process; Add 30L 80 DEG C of hot water again, controlled circulation pump discharge 125L/h soak cycles washing 8-24h, every half an hour, hot water is sampled in circulation flushing process, after water muddiness is dirty, addle is discharged and again fill into 80 DEG C of hot water continuation circulation flushings, as clear as crystal for terminal with sampling water; After the catalyst emptying hot water after circulation flushing, then use 60 DEG C, 30 DEG C deionized water circular treatment twice respectively, fixed bed temperature is down to 30-40 DEG C, then water is put only; The catalyst cooling the temperature to 30-40 DEG C draws off from fixed bed, wash after soaking half an hour with 20-50 DEG C of aromatic hydrocarbons, period, available wooden rake stirred, catalyst if any caking need by cake broke, be washed till catalyst surface bright and clean without till organic addendum, catalyst is put into the dry aromatic hydrocarbons in stainless steel mesh overhead afterwards, with after the new working solution of the recyclable preparation of aromatic hydrocarbons or directly fill into system; By the catalyst 30-50 of dry for sky aromatic hydrocarbons DEG C of deionized water washing, after washes clean, catalyst taking-up is put into the empty solid carbon dioxide of stainless steel mesh and divides; The catalyst that empty solid carbon dioxide divides is shakeout airing on clean Polypropylence Sheet, dries loading clean packaging bag (plastic lining film) interior tying after sieving and put well; After whole catalyst treatment, catalyst is backfilling into hydrogenation tower again, the qualified rear nitrogen displacement of hydrogenation tower leak test, slowly passes into Hydrogen activation after nitrogen displacement is qualified, and activation temperature controls within room temperature ~ 80 DEG C; After activation, sampling is surveyed active, hydrogenation efficiency 8.0g/L.
Embodiment 4
Get and need regenerate palladium catalyst 10Kg loading regenerating unit, add the aromatic hydrocarbons of 30L50 DEG C, controlled circulation pump discharge 125L/h soak cycles washing 8h, then drains recovery by aromatic hydrocarbons; Pass into the saturated steam process 16h-48h of 100-120 DEG C again, as clear as crystal for terminal with steam condensate (SC).Saturated steam steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, reuses in initial stage steam condensate (SC) containing some work liquid is recyclable after alkali cleaning washing process; Add 30L95 DEG C of hot water again, controlled circulation pump discharge 125L/h soak cycles washing 8-24h, every half an hour, hot water is sampled in circulation flushing process, after water muddiness is dirty, addle is discharged and again fill into 95 DEG C of hot water continuation circulation flushings, as clear as crystal for terminal with sampling water; After the catalyst emptying hot water after circulation flushing, cooling catalyst is drawn off to 30-40 DEG C from fixed bed, wash after soaking half an hour with 20-50 DEG C of aromatic hydrocarbons, be washed till that catalyst surface is bright and clean without organic addendum is, catalyst is put into the dry aromatic hydrocarbons in stainless steel mesh overhead afterwards; By the washing of the catalyst 30-50 of dry for sky aromatic hydrocarbons DEG C of deionized water, be washed till catalyst surface bright and clean without inorganic attach thing till, afterwards catalyst is taken out and is put into the empty solid carbon dioxide of stainless steel mesh and divides; The catalyst that empty solid carbon dioxide divides is shakeout airing on clean Polypropylence Sheet, after drying, catalyst is backfilling into regenerating unit, the qualified rear nitrogen of device leak test is replaced, slowly Hydrogen activation is passed into after nitrogen displacement is qualified, within activation temperature controls room temperature-80 DEG C, after activation, sampling is surveyed active, hydrogenation efficiency 8.2g/L.
Comparative example 1
Get and need regenerate palladium catalyst 10Kg loading regenerating unit, add the aromatic hydrocarbons of 30L50 DEG C, controlled circulation pump discharge 125L/h soak cycles washing 16h, then drains recovery by aromatic hydrocarbons, draws off catalyst sampling and surveys active, hydrogenation efficiency 6.3g/L.
Comparative example 2
Get and need regenerate palladium catalyst 10Kg loading regenerating unit, pass into the saturated steam process 16h-48h of 100-120 DEG C, as clear as crystal for terminal with steam condensate (SC).Saturated steam steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, reuse after alkali cleaning washing process containing some work liquid is recyclable in initial stage steam condensate (SC), pass into 100-150 DEG C of hot nitrogen after steam treated catalyst is dried up, catalyst dries up rear maintenance positive pressure of nitrogen atmosphere and slowly passes into hydrogen and carry out activation process to catalyst, within activation temperature controls room temperature-80 DEG C, after activation, sampling is surveyed active, hydrogenation efficiency 6.2g/L.
Comparative example 3
Get and need regenerate palladium catalyst 10Kg loading regenerating unit, add the aromatic hydrocarbons of 30L50 DEG C, controlled circulation pump discharge 125L/h soak cycles washing 8h, then drains recovery by aromatic hydrocarbons; Pass into the saturated steam process 16h-48h of 100-120 DEG C again, as clear as crystal for terminal with steam condensate (SC).Saturated steam steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, reuses in initial stage steam condensate (SC) containing some work liquid is recyclable after alkali cleaning washing process; Pass into 100-150 DEG C of hot nitrogen after steam treated again catalyst is dried up, catalyst dries up rear maintenance positive pressure of nitrogen atmosphere and slowly passes into hydrogen and carry out activation process to catalyst, within activation temperature controls room temperature-80 DEG C, after activation, sampling is surveyed active, hydrogenation efficiency 6.6g/L.
Comparative example 4
Need regenerated catalyst to sample and survey activity, hydrogenation efficiency 5.2g/L.
Comparative example 5
Raw catelyst sampling is surveyed active, hydrogenation efficiency 8.3g/L.
Embodiment 1-4 and comparative example 1-5 shows, process catalyst according to the inventive method regeneration process catalyst than with conventional method regeneration, regenerated catalyst activation recovering is better, and reducing production cost to extending catalyst life cycle and service life has positive role.
Above embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that the common engineers and technicians in this area make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (5)
1. a renovation process for the palladium catalyst of hydrogen dioxide solution production by anthraquinone process, is characterized in that it comprises the steps:
A) will the catalyst of regeneration be needed to soak 8-16 hour with the aromatic hydrocarbons of 30-70 DEG C in device or pass through circulating pump circulation flushing 8-16 hour with the aromatic hydrocarbons of 30-70 DEG C; Aromatic hydrocarbons addition is as the criterion with complete submergence catalyst;
B) catalyst is with the saturated steam process 16-48h of 100-120 DEG C in device, and wherein steam consumption is advisable with catalyst per ton consumption per hour 0.2-0.5 ton, as clear as crystal for terminal with steam condensate (SC);
C) catalyst passes through circulating pump circulation flushing 8-24h with 30-95 DEG C of hot-water soak 8-24h or with 30-95 DEG C of hot water in device, soak or every half an hour, hot water sampled in circulation flushing process, after water muddiness is dirty, addle is discharged and again fill into 30-95 DEG C of hot water continuation immersion or circulation flushing, as clear as crystal for terminal with sampling water;
D) catalyst after above-mentioned immersion or circulation flushing carries out nitrogen displacement, Hydrogen activation process, and within activation temperature controls room temperature ~ 80 DEG C, catalyst activation is complete can come into operation again.
2. the renovation process of the palladium catalyst of a kind of hydrogen dioxide solution production by anthraquinone process according to claim 1, it is characterized in that after the catalyst emptying hot water after immersion or circulation flushing in described step d), pass into 100-150 DEG C of hot nitrogen catalyst is dried up, catalyst dries up rear maintenance positive pressure of nitrogen atmosphere and slowly passes into hydrogen and carry out activation process to catalyst, within activation temperature controls room temperature ~ 80 DEG C, catalyst activation is complete can come into operation again.
3. the renovation process of the palladium catalyst of a kind of hydrogen dioxide solution production by anthraquinone process according to claim 1, it is characterized in that after the catalyst emptying hot water after immersion or circulation flushing in described step d), cooling catalyst is drawn off to 30-40 DEG C from fixed bed, wash after soaking half an hour with 20-50 DEG C of aromatic hydrocarbons, be washed till catalyst surface bright and clean without till organic addendum, catalyst is put into the dry aromatic hydrocarbons in stainless steel mesh overhead afterwards, by the catalyst 30-50 of dry for sky aromatic hydrocarbons DEG C of deionized water washing, after washes clean, catalyst taking-up is put into the empty solid carbon dioxide of stainless steel mesh to divide, afterwards catalyst is dried, dry packaging after sieving to put well, after whole catalyst treatment, catalyst is backfilling into hydrogenation tower again, the qualified rear nitrogen of hydrogenation tower leak test is replaced, slowly Hydrogen activation is passed into after nitrogen displacement is qualified, within activation temperature controls room temperature-80 DEG C, catalyst activation is complete can come into operation again.
4. the renovation process of the palladium catalyst of a kind of hydrogen dioxide solution production by anthraquinone process according to claim 3, it is characterized in that described will immersion or after catalyst emptying hot water after circulation flushing, use 60 DEG C, 30 DEG C deionized water circular treatment twice more respectively, fixed bed temperature is down to 30-40 DEG C, then water is put only; The catalyst cooling the temperature to 30-40 DEG C draws off from fixed bed.
5. the renovation process of the palladium catalyst of a kind of hydrogen dioxide solution production by anthraquinone process according to claim 1, is characterized in that in described step c), hot water temperature is 80-95 DEG C.
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| CN106268864B (en) * | 2016-09-22 | 2019-07-16 | 福建省福大百阳化工科技有限公司 | A kind of regeneration method of palladium catalyst |
| CN107298454A (en) * | 2017-08-01 | 2017-10-27 | 广西壮族自治区化工研究院 | A kind of method for preparing activated alumina using discarded anthraquinone regenerative agent |
| CN107298454B (en) * | 2017-08-01 | 2019-02-22 | 广西壮族自治区化工研究院 | A method of activated alumina is prepared using discarded anthraquinone regenerative agent |
| CN110980654B (en) * | 2019-12-30 | 2023-04-14 | 广西田东达盛化工科技有限公司 | Method for cleaning active alumina balls in hydrogen peroxide production |
| CN110980654A (en) * | 2019-12-30 | 2020-04-10 | 广西田东达盛化工科技有限公司 | Method for cleaning active alumina balls in hydrogen peroxide production |
| CN111437889A (en) * | 2020-04-01 | 2020-07-24 | 安徽泉盛化工有限公司 | Regeneration method of catalyst of hydrogenation system for producing hydrogen peroxide by anthraquinone process |
| CN115430421A (en) * | 2021-06-01 | 2022-12-06 | 中国石油化工股份有限公司 | Preparation method of anthraquinone hydrogenation catalyst |
| CN115430465A (en) * | 2021-06-01 | 2022-12-06 | 中国石油化工股份有限公司 | Regeneration method of anthraquinone hydrogenation catalyst |
| CN115430465B (en) * | 2021-06-01 | 2024-01-05 | 中国石油化工股份有限公司 | Regeneration method of anthraquinone hydrogenation catalyst |
| CN115430421B (en) * | 2021-06-01 | 2024-01-09 | 中国石油化工股份有限公司 | Preparation method of anthraquinone hydrogenation catalyst |
| CN113289694A (en) * | 2021-06-28 | 2021-08-24 | 广西田东达盛化工科技有限公司 | Method for regenerating palladium catalyst in production of hydrogen peroxide by anthraquinone process |
| CN114887669A (en) * | 2022-03-10 | 2022-08-12 | 中国平煤神马集团尼龙科技有限公司 | Regeneration method of catalyst for producing hydrogen peroxide by anthraquinone process |
| CN117380183A (en) * | 2023-12-04 | 2024-01-12 | 黎明化工研究设计院有限责任公司 | Preparation method and application of supported palladium nanoparticle catalyst |
| CN117380183B (en) * | 2023-12-04 | 2024-02-20 | 黎明化工研究设计院有限责任公司 | Preparation method and application of supported palladium nanoparticle catalyst |
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