CN104841410B - Ammonia water pretreatment resurrection method of S-Zorb waste adsorbent - Google Patents
Ammonia water pretreatment resurrection method of S-Zorb waste adsorbent Download PDFInfo
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- CN104841410B CN104841410B CN201510325982.6A CN201510325982A CN104841410B CN 104841410 B CN104841410 B CN 104841410B CN 201510325982 A CN201510325982 A CN 201510325982A CN 104841410 B CN104841410 B CN 104841410B
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Abstract
The invention relates to an ammonia water pretreatment resurrection method of an S-Zorb waste adsorbent, and belongs to the field of treatment and application of solid wastes. The ammonia water pretreatment resurrection method of the S-Zorb waste adsorbent comprises the following steps: mixing and stirring an ammonia water solution and the S-Zorb waste adsorbent, washing and filtering through deionized water, drying, and roasting for 0.5-4 hours at 350-600 DEG C to obtain a resurrected adsorbent. Through the adoption of the S-Zorb waste adsorbent resurrection method provided by the invention, the S-Zorb waste adsorbent is treated through the ammonia water, the waste adsorbent is chemically treated through a chemical method, and the structure and chemical components of the waste adsorbent are fundamentally changed, so that the adsorbent is resurrected, the resurrection method is simple and flexible in operation, the waste adsorbent is efficiently recycled, the pressure of three-wastes treatment of an enterprise is relieved, the specific surface area and the pore volume of the resurrected S-Zorb waste adsorbent are greatly increased, and the adsorption desulfurization performance is good.
Description
Technical field
The present invention relates to the pretreatment with agueous Ammonia rejuvenation method of S-Zorb spent sorbents, belong to the treatment of solid waste and answer
Use field.
Background technology
Increasingly strict with environmental regulation, requirement of the China to content of sulfur in gasoline is more and more stricter, will in National V emission standard
Content of sulfur in gasoline is sought less than 10ppm, and S-Zorb techniques are deep desulfurization of gasoline technology, can produce satisfactory gasoline.
Adsorbent major part in current S-Zorb techniques still relies on import, and Sinopec has been developed meeting China
The adsorbent of production technology and apply for a patent, the domestic Home-produced Reconstruction to S-Zorb techniques also causes that the technique is increasingly fitted
Close Chinese raw material.But whether how technique domesticizes, substantial amounts of spent sorbents can be all produced.Such as Qilu Petrochemical, annual 90
Ten thousand tons of scale, spent sorbents amount is about 45 tons, and its expense accounts for the 18.23% of unit mass gasoline production cost.So the work
The Industry Waste quantity of sorbent that skill is produced is still very big, if the spent sorbents are all processed as waste, wherein what is contained has
Effect nickel, zinc isoreactivity component are lost in than larger, and discarded object landfill can take substantial amounts of land resource, can be with into soil
Natural Circulation enters in water, can cause the pollution of soil and water resource, brings serious environmental problem, the life of the serious threat mankind
Dis environment.
It is fewer to the research of the recycling of S-Zorb spent sorbents at present, physiochemical mutagens are concentrated mainly on such as with rotation
Wind separator or Magneto separate.This mode is that will wherein meet the material of certain granules size or only will wherein have magnetic
Nickel separate, it is impossible to it is real to accomplish so that spent sorbents regenerate.
The content of the invention
For above-mentioned technical problem, the present invention provides a kind of rejuvenation method of S-Zorb spent sorbents, realizes spent sorbents
Regeneration.
Concrete technical scheme is：
The pretreatment with agueous Ammonia rejuvenation method of S-Zorb spent sorbents, comprises the following steps：
(1) it is 2 according to liquid-solid ratio by ammonia spirit and S-Zorb spent sorbents:1~8:1 ratio, at room temperature mixing is stirred
Mix 3~10 hours, be then washed with deionized and filter, deionized water and S-Zorb spent sorbents mass ratio are 6:1~10:
1, then the adsorbent for obtaining for 1~6 hour tentatively regenerating through 60~150 DEG C of dryings；
(2) adsorbent after preliminary regeneration is calcined 0.5~4 hour at 350~600 DEG C, obtains bringing back to life adsorbent.
The mass concentration of the ammonia spirit described in step (1) is 5%~20%.
The S-Zorb spent sorbents rejuvenation methods that the present invention is provided, using AMMONIA TREATMENT S-Zorb spent sorbents, with chemistry
Method is chemically treated to spent sorbents, can fundamentally change the structure and chemical constituent of spent sorbents, accomplishes to make suction
Attached dose of resurrection, rejuvenation method is simple, and operation is flexible, and spent sorbents are carried out with efficient reuse, mitigates the pressure of enterprise's disposal of waste gas, water and industrial residue
Power, S-Zorb spent sorbents specific surface area and pore volume after resurrection are increased considerably, and absorption desulfurization performance is good.
Specific embodiment
It is described in conjunction with the embodiments specific embodiment of the invention.
Embodiment 1
It is 8 according to solid-to-liquid ratio with S-Zorb spent sorbents by the ammonia spirit that mass concentration is 5%:1 ratio, at room temperature
Mix 10 hours, adsorbent is washed with deionized water then, the quality of deionized water and S-Zorb spent sorbents
Than being 6:1, measured with the butt of S-Zorb spent sorbents；Again the preliminary absorption for regenerating is obtained within 3 hours through filtering and 120 DEG C of dryings
Agent, the adsorbent after preliminary regeneration is carried out being calcined 2.5 hours at 450 DEG C, obtains bringing back to life adsorbent.
S-Zorb device of the S-Zorb spent sorbents from Sinopec Qilu Petrochemical Company 0.9Mt/a.
Embodiment 2
It is 5 according to solid-to-liquid ratio with S-Zorb spent sorbents by the ammonia spirit that mass concentration is 10%:1 ratio is at room temperature
Mix 7 hours, adsorbent is washed with deionized water then, the mass ratio of deionized water and S-Zorb spent sorbents
It is 8:1, then the preliminary adsorbent for regenerating is obtained within 4 hours through filtering and 100 DEG C of dryings, the adsorbent after preliminary regenerating is 500
Carry out being calcined 1.5 hours at DEG C, obtain bringing back to life adsorbent.
Embodiment 3
It is 2 according to solid-to-liquid ratio with S-Zorb spent sorbents by the ammonia spirit that mass concentration is 20%:1 ratio, room temperature
It is lower to mix 3 hours, adsorbent is washed with deionized water then, the quality of deionized water and S-Zorb spent sorbents
Than being 10:1, then the preliminary adsorbent for regenerating is obtained within 2 hours through filtering and 150 DEG C of dryings, the adsorbent after preliminary regeneration is existed
Carry out being calcined 0.5 hour at 600 DEG C, obtain bringing back to life adsorbent.
Embodiment 4
It is 4 according to solid-to-liquid ratio with S-Zorb spent sorbents by the ammonia spirit that mass concentration is 15%:1 ratio, room temperature
It is lower to mix 5 hours, adsorbent is washed with deionized water then, the quality of deionized water and S-Zorb spent sorbents
Than being 9:1, then the preliminary adsorbent for regenerating is obtained within 5 hours through filtering and 80 DEG C of dryings, the adsorbent after preliminary regenerating is 350
Carry out being calcined 4 hours at DEG C, obtain bringing back to life adsorbent.
Embodiment 5
It is 7 according to solid-to-liquid ratio with S-Zorb spent sorbents by the ammonia spirit that mass concentration is 8%:1 ratio, at room temperature
Mix 8 hours, adsorbent is washed with deionized water then, the mass ratio of deionized water and S-Zorb spent sorbents
It is 7:1, then the preliminary adsorbent for regenerating is obtained within 6 hours through filtering and 60 DEG C of dryings, the adsorbent after preliminary regenerating is at 550 DEG C
Under carry out be calcined 1 hour, obtain bring back to life adsorbent.
S-Zorb adsorbents specific surface and hole body after the former agent of S-Zorb spent sorbents and the above each embodiment resurrection
Volume data is specifically shown in Table 1, and desulfurization performance evaluation result is shown in Table 2.
The S-Zorb of table 1 brings back to life adsorbent physical and chemical performance
| Project | Specific surface (m2/g) | Pore volume (cm3/g) |
| Former agent | 28.9 | 0.065 |
| Embodiment 1 | 78.5 | 0.198 |
| Embodiment 2 | 71.1 | 0.128 |
| Embodiment 3 | 71.9 | 0.134 |
| Embodiment 4 | 64.6 | 0.131 |
| Embodiment 5 | 61.2 | 0.115 |
The S-Zorb of table 2 brings back to life adsorbent desulfurization performance evaluation result
| Project | Sulfur content in gasoline (μ g/g) after absorption desulfurization | Desulfurization degree (%) |
| Former agent | 142.7 | 81.17 |
| Embodiment 1 | 2.8 | 99.63 |
| Embodiment 2 | 7.9 | 98.96 |
| Embodiment 3 | 16.5 | 97.82 |
| Embodiment 4 | 12.7 | 98.32 |
| Embodiment 5 | 23.4 | 96.91 |
Adsorbent specific surface area and pore volume are determined using BET method, referring to《Petrochemical Engineering Analysis method (RIPP experiment sides
Method)》, RIPP151-90 methods, Science Press, nineteen ninety September.Determining instrument is the production of Micromeritics companies
The multi-functional adsorption instrument of TriStar3000 types.
It is to the actual conditions for bringing back to life adsorbent HDS evaluation in example：Gained is brought back to life into adsorbent grinding, compressing tablet to be made
The particle of 20~60 mesh, the loading of adsorbent is 3ml, and pre-reduction temperature is 395 DEG C, and pressure is 0.5MPa, hydrogen flowing quantity
20ml/min, the recovery time is 4 hours.HDS evaluation condition：350 DEG C of temperature, pressure 0.5MPa, air speed 2.0h-1, hydrogen oil volume
Than 200: 1, stabilization takes the product of the 5th hour, and sulfur-free gasoline is Zhongyuan Oil Field general petrochemicals factory catalytically cracked gasoline, and sulfur content is
757.8μg/g。
Claims (2)
- The pretreatment with agueous Ammonia rejuvenation method of 1.S-Zorb spent sorbents, it is characterised in that comprise the following steps：(1) it is 2 according to liquid-solid ratio by ammonia spirit and S-Zorb spent sorbents:1~8:1 ratio, at room temperature mix 3~ 10 hours, then it is washed with deionized and filters, deionized water and S-Zorb spent sorbents mass ratio is 6:1~10:1, then Through the adsorbent that 60~150 DEG C of dryings obtain tentatively regenerating for 1~6 hour；(2) adsorbent after preliminary regeneration is calcined 0.5~4 hour at 350~600 DEG C, obtains bringing back to life adsorbent.
- 2. the pretreatment with agueous Ammonia rejuvenation method of S-Zorb spent sorbents according to claim 1, it is characterised in that step (1) the ammonia spirit mass concentration described in is 5%~20%.
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| CN104841410B true CN104841410B (en) | 2017-05-24 |
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Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US7091152B2 (en) * | 2003-01-24 | 2006-08-15 | Conocophillips Company | Catalyst composition comprising a heteropoly acid, zinc, and a support component and processes therefor and therewith |
| CN102836699A (en) * | 2012-09-24 | 2012-12-26 | 北京立诚石化技术有限公司 | Regenerating and recycling system and method for S-Zorb waste absorbing agent |
| CN104084041B (en) * | 2014-07-17 | 2016-08-17 | 北京三聚创洁科技发展有限公司 | A kind of zinc oxide desulfurization gives up the renovation process of agent |
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