Regeneration method of sulfonated kerosene-containing granular carbon

Abstract

The invention relates to a regeneration method of sulfonated kerosene-containing granular carbon, and belongs to the technical field of regeneration methods. The regeneration method comprises the following steps: preparing activated carbon containing sulfonated kerosene, wherein the adsorption amount of the sulfonated kerosene is 5-20wt% based on the dry weight of the activated carbon; the sulfonated kerosene-containing activated carbon is placed in drying equipment and is dried at the temperature of 80-120 DEG C for 1-3 h; transferring the dried sulfonated kerosene-containing activated carbon into a regeneration furnace, and carrying out regeneration treatment at 200-350 DEG C in an inert gas protection atmosphere for 2-4 hours; and after the regeneration treatment is finished, stopping heating, and naturally cooling to room temperature in an inert gas atmosphere to obtain regenerated activated carbon. No chemical reagent is used in the whole process, so that secondary pollution is avoided; in addition, efficient regeneration of granular carbon is achieved, and the prominent problem of resource waste in an existing treatment method is thoroughly solved.

Description

Technical Field

[0001] This invention relates to the technical field of regeneration methods, and specifically to a regeneration method for carbon containing sulfonated kerosene particles. Background Technology

[0002] Sulfonated kerosene is a special solvent obtained by sulfonating and refining straight-run kerosene. Its core function is to remove unsaturated impurities such as aromatics and olefins, thereby improving chemical stability and extraction performance. During the production of sulfonated kerosene, particulate carbon is easily generated during the sulfonation reaction and distillation stages. The proper treatment and resource recovery of this particulate carbon-containing sulfonated kerosene has become an important issue of current industry concern.

[0003] There are two main methods for treating sulfonated kerosene containing particulate carbon. The first method is biomass fuel conversion, which uses the sulfonated kerosene as biomass fuel in an incinerator. This method only releases energy in a single step and cannot recover the effective components from the sulfonated kerosene and particulate carbon, making it difficult to achieve resource recycling. Furthermore, the incineration process easily generates harmful gases and other pollutants, causing significant negative impacts on the ecological environment. The second method is chemical regeneration, which regenerates the sulfonated kerosene through the action of chemical reagents. However, chemical regeneration requires large amounts of expensive chemical reagents, resulting in high regeneration costs. Additionally, the regeneration reaction produces a large amount of chemical residue, which, if not properly treated, can easily cause secondary pollution problems such as soil and water pollution, hindering environmentally friendly development.

[0004] In summary, existing treatment methods suffer from drawbacks such as low raw material utilization, significant environmental impact, high treatment costs, and the potential for secondary pollution. A more optimized treatment technology is urgently needed to address these issues. Summary of the Invention

[0005] To address the existing technical problems of low raw material utilization and easy secondary pollution in the processing of sulfonated kerosene containing particulate carbon, this invention provides a method for regenerating particulate carbon in sulfonated kerosene to solve the above problems.

[0006] The technical solution of this invention is as follows: A method for regenerating carbon particles containing sulfonated kerosene includes the following steps: (1) Raw material preparation steps: Prepare activated carbon containing sulfonated kerosene. The activated carbon containing sulfonated kerosene is a mixture of particulate carbon that adsorbs sulfonated kerosene during the use of sulfonated kerosene. The amount of sulfonated kerosene adsorbed is 5wt%~20wt% based on the dry weight of the activated carbon.

[0007] (2) Drying process: The activated carbon containing sulfonated kerosene is placed in a drying device and dried at 80℃~120℃ for 1~3 hours. Using a temperature range of 80℃~120℃, which is lower than the boiling point of sulfonated kerosene (approximately 180℃~310℃), allows for efficient removal of free water and a small amount of surface-adsorbed light impurities from the raw material, while avoiding premature desorption of the sulfonated kerosene. If the temperature is below 80℃, the water removal efficiency will be low, leading to mixing of water and sulfonated kerosene during subsequent regeneration, affecting the recovery quality of the sulfonated kerosene. If the temperature is above 120℃, it may cause localized volatilization of the sulfonated kerosene, resulting in energy waste and internal equipment contamination. Simultaneously, the 1~3 hour drying time, combined with a vacuum environment, can reduce the moisture content of the raw material to below 0.5%, creating a dry environment for efficient desorption of the sulfonated kerosene in subsequent regeneration steps and preventing water from interfering with the regeneration reaction.

[0008] (3) Regeneration process: The dried activated carbon containing sulfonated kerosene is transferred to a regeneration furnace and regenerated at 200℃~350℃ under an inert gas protective atmosphere for 2~4 hours. Sulfonated kerosene has a wide flammability limit, usually between 0.6% and 7.5%, while its vapor pressure is low, usually between 1.5 and 10 kPa. The temperature range of 200℃~350℃ is the desorption temperature range of sulfonated kerosene. At this temperature, sulfonated kerosene can be fully desorbed from the pore structure of particulate carbon without causing ablation or structural damage due to excessive temperature. If the temperature is below 200℃, the sulfonated kerosene desorption is incomplete, and the adsorption performance of the particulate carbon cannot be effectively restored; if the temperature is above 350℃, the specific surface area of ​​the particulate carbon will decrease due to high-temperature sintering, resulting in a decline in the performance of the regenerated product. Furthermore, sulfonated kerosene has strong oxidizing properties, which can easily lead to fires and explosions. Therefore, the regeneration system is set to an inert gas atmosphere. This prevents the sulfonated kerosene produced during desorption from oxidizing and deteriorating upon contact with air, facilitating its subsequent recycling and reuse, thus achieving resource recycling. On the other hand, it prevents the particulate carbon from being oxidized and burned at high temperatures, ensuring a high recovery rate of particulate carbon after regeneration (over 95%). The regeneration time of 2-4 hours, combined with the gas flow rate, ensures complete desorption of the sulfonated kerosene from the pores of the particulate carbon, restoring the adsorption capacity of the regenerated activated carbon to over 90% of that of new carbon.

[0009] (4) Cooling Step: After the regeneration process is completed, heating is stopped, and the activated carbon is naturally cooled to room temperature under an inert gas atmosphere to obtain regenerated activated carbon. The cooling step, performed naturally under an inert gas atmosphere, avoids oxidation of the regenerated activated carbon at high temperatures upon contact with air, and also prevents moisture in the air from being re-adsorbed onto the surface of the granular carbon. Natural cooling to room temperature avoids cracking of the granular carbon due to sudden cooling, ensuring the integrity of the physical structure of the regenerated activated carbon and guaranteeing its good mechanical properties and adsorption stability. The regenerated activated carbon obtained after cooling can be directly used for subsequent adsorption operations without additional processing, simplifying the production process.

[0010] Furthermore, the particle size of the sulfonated kerosene activated carbon in step (1) is 0.1~1mm, which ensures that heat can be evenly transferred to the interior of the particles during subsequent drying and regeneration processes, and avoids incomplete local treatment.

[0011] Furthermore, in step (1), the bulk density of the activated carbon is 0.5 t / m³. 3 The moisture content of the wet activated carbon is 40%.

[0012] Furthermore, in step (1), the water content of the sulfonated kerosene activated carbon is 30%~40%.

[0013] Furthermore, in step (2), the drying equipment is a vacuum drying box with a vacuum degree controlled at -0.08~-0.05MPa. The vacuum environment can accelerate the volatilization of free water and some low-boiling-point light components in activated carbon containing sulfonated kerosene, shorten the drying time, and at the same time avoid premature oxidation of sulfonated kerosene at high temperature.

[0014] Furthermore, in step (3), the inert gas is nitrogen or argon, and the gas flow rate is controlled at 0.5~2L / min. The inert gas atmosphere can isolate the air and prevent the particulate carbon and desorbed sulfonated kerosene from oxidizing and burning during the regeneration process, ensuring the safety of the regeneration process. At the same time, it can carry out the sulfonated kerosene vapor generated by desorption in time, promoting the positive shift of the desorption equilibrium.

[0015] Furthermore, in step (4), the inert gas is nitrogen or argon.

[0016] Furthermore, in step (2), the moisture content of the dried sulfonated kerosene activated carbon is <0.5%.

[0017] Furthermore, in step (4), the flow rate of the inert gas is controlled to be 0.5~2L / min.

[0018] The beneficial effects of this invention are as follows: Compared with existing technologies, the regeneration method for sulfonated kerosene-containing particulate carbon does not use chemical reagents throughout the entire process, fundamentally avoiding the secondary pollution problems caused by chemical residues in chemical regeneration methods. Simultaneously, the segmented temperature-controlled treatment under inert gas protection effectively avoids the emission risks of harmful gases associated with incineration methods, making it more environmentally friendly. This invention not only achieves highly efficient regeneration of particulate carbon, restoring the adsorption capacity of the regenerated particulate carbon to over 90% of that of new carbon with a recovery rate exceeding 95%, but also simultaneously recovers sulfonated kerosene with a purity higher than 97%, successfully realizing the recycling of two core resources and completely solving the prominent problem of resource waste in existing treatment methods. Furthermore, the process steps of this invention are simple, requiring no investment in expensive chemical reagents and supporting wastewater treatment equipment. The regeneration process can be completed simply by adjusting the temperature and inert gas flow rate. The equipment investment and operating costs are significantly lower than those of chemical regeneration methods. Compared with incineration methods, it can create additional economic benefits through resource recovery, resulting in a clear overall cost advantage. In terms of ease of operation, the process parameters of each step of this invention are highly controllable, adaptable to the raw material processing needs of different sulfonated kerosene adsorption capacities, and the regenerated product has stable performance. It can be put into use without complicated subsequent debugging, facilitating large-scale industrial application. Detailed Implementation

[0019] To enable those skilled in the art to better understand the technical solutions of this invention, the technical solutions in the embodiments of this invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of this invention, and not all embodiments. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of this invention.

[0020] Example 1 A method for regenerating carbon particles containing sulfonated kerosene includes the following steps: (1) Raw material preparation: Select activated carbon containing sulfonated kerosene with an adsorption capacity of 10% (mass fraction) and a particle size of 0.3~0.5mm as raw material.

[0021] (2) Drying treatment: The raw material is placed in a vacuum drying oven, the vacuum degree is set to -0.07MPa, the temperature is 100℃, the drying time is 2h, and the moisture content of the raw material after drying is 0.3%.

[0022] (3) Regeneration treatment: The dried raw material is transferred to a tubular regeneration furnace, nitrogen is introduced as an inert protective gas with a flow rate of 1L / min, the temperature is raised to 300℃, and the temperature is maintained for 3h for regeneration treatment.

[0023] (4) Cooling treatment: Stop heating and continue to introduce nitrogen until the raw material cools naturally to room temperature to obtain regenerated activated carbon.

[0024] Testing showed that the recovery rate of the regenerated activated carbon prepared in Example 1 was 96.2%, the adsorption capacity was 92.5% of that of the new activated carbon, and the purity of the sulfonated kerosene obtained by desorption was 98.1%, which can be directly reused in industrial production.

[0025] Example 2 A method for regenerating carbon particles containing sulfonated kerosene includes the following steps: (1) Raw material preparation: Select activated carbon containing sulfonated kerosene with an adsorption capacity of 5% (mass fraction) and a particle size of 0.1~0.3mm as raw material.

[0026] (2) Drying treatment: The raw material is placed in a vacuum drying oven, the vacuum degree is set to -0.05MPa, the temperature is 80℃, the drying time is 3h, and the moisture content of the raw material after drying is 0.4%.

[0027] (3) Regeneration treatment: The dried raw material is transferred to a tubular regeneration furnace, and argon gas is introduced as an inert protective gas with a flow rate of 0.5 L / min. The temperature is raised to 200℃ and kept at this temperature for 4 hours for regeneration treatment.

[0028] (4) Cooling treatment: Stop heating and continue to introduce argon gas until the raw material cools naturally to room temperature to obtain regenerated activated carbon.

[0029] Testing showed that the recovery rate of the regenerated activated carbon prepared in Example 2 was 95.8%, the adsorption capacity was 90.3% of that of the new activated carbon, and the purity of the sulfonated kerosene obtained from desorption was 97.8%, which can be directly reused in industrial production.

[0030] Example 3 A method for regenerating carbon particles containing sulfonated kerosene includes the following steps: (1) Raw material preparation: Select activated carbon containing sulfonated kerosene with an adsorption capacity of 20% (mass fraction) and a particle size of 0.5~1mm as raw material.

[0031] (2) Drying treatment: The raw material is placed in a vacuum drying oven, the vacuum degree is set to -0.08MPa, the temperature is 120℃, the drying time is 1h, and the moisture content of the raw material after drying is 0.2%.

[0032] (3) Regeneration treatment: The dried raw material is transferred to a tubular regeneration furnace, and nitrogen is introduced as an inert protective gas with a flow rate of 2L / min. The temperature is raised to 350℃ and kept at this temperature for 2 hours for regeneration treatment.

[0033] (4) Cooling treatment: Stop heating and continue to introduce nitrogen until the raw material cools naturally to room temperature to obtain regenerated activated carbon.

[0034] Testing showed that the recovery rate of the regenerated activated carbon prepared in Example 3 was 96.5%, the adsorption capacity was 93.1% of that of the new activated carbon, and the purity of the sulfonated kerosene obtained from desorption was 98.3%, which can be directly reused in industrial production.

[0035] Although the present invention has been described in detail by way of preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made to the embodiments of the present invention by those skilled in the art without departing from the spirit and essence of the invention, and such modifications or substitutions should all be within the scope of the present invention. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should also be covered within the protection scope of the present invention.

Claims

1. A method for regenerating carbon particles containing sulfonated kerosene, characterized in that, Includes the following steps: (1) Raw material preparation steps: Prepare activated carbon containing sulfonated kerosene. The activated carbon containing sulfonated kerosene is a mixture of granular carbon that has adsorbed sulfonated kerosene during the use of sulfonated kerosene. The amount of sulfonated kerosene adsorbed is 5 wt% to 20 wt% based on the dry weight of the activated carbon. (2) Drying process: Place the activated carbon containing sulfonated kerosene in a drying device and dry it at 80℃~120℃ for 1~3 hours. (3) Regeneration process: The dried activated carbon containing sulfonated kerosene is transferred to a regeneration furnace and regenerated at 200℃~350℃ under an inert gas protective atmosphere for 2~4 hours. (4) Cooling step: After the regeneration process is completed, stop heating and allow it to cool naturally to room temperature under an inert gas atmosphere to obtain regenerated activated carbon.

2. The method for regenerating carbon containing sulfonated kerosene particles as described in claim 1, characterized in that, The particle size of the sulfonated kerosene activated carbon mentioned in step (1) is 0.1~1mm.

3. The method for regenerating carbon containing sulfonated kerosene particles as described in claim 1, characterized in that, In step (1), the bulk density of the sulfonated kerosene activated carbon is 0.5 t / m³. 3 .

4. The method for regenerating sulfonated kerosene particulate carbon as described in claim 1, characterized in that, In step (1), the water content of the sulfonated kerosene activated carbon is 30%~40%.

5. The method for regenerating carbon containing sulfonated kerosene particles as described in claim 1, characterized in that, In step (2), a vacuum drying oven is used as the drying equipment, and the vacuum degree is controlled at -0.08~-0.05MPa.

6. The method for regenerating carbon containing sulfonated kerosene particles as described in claim 1, characterized in that, In step (3), the inert gas is nitrogen or argon.

7. The method for regenerating carbon containing sulfonated kerosene particles as described in claim 1, characterized in that, In step (4), the inert gas is nitrogen or argon.

8. The method for regenerating sulfonated kerosene particulate carbon as described in claim 1, characterized in that, In step (2), the moisture content of the dried sulfonated kerosene activated carbon is <0.5%.

9. The method for regenerating sulfonated kerosene particulate carbon as described in claim 1, characterized in that, In step (3), the flow rate of the inert gas is controlled to be 0.5~2L / min.