System for step-by-step separation and conversion of tar residues

Abstract

The utility model discloses a system for step-by-step separation and conversion of tar residues, which comprises an ultrasonic cleaning instrument, the liquid outlet end of the ultrasonic cleaning instrument is connected with a solid-liquid separator through a pipeline, the liquid outlet end of an upper liquid layer of the solid-liquid separator is connected with a delivery pump I through a pipeline, and the delivery pump I is connected with the liquid inlet end of a rotary evaporator I through a pipeline. Concentrated organic matters in the rotary evaporator I are conveyed into a vertically arranged chromatographic column through a pipeline, the lower end of the chromatographic column is connected with a sand core funnel, a collecting tank is placed below an outlet of the sand core funnel, the collecting tank is connected with a conveying pump V through a pipeline, and the conveying pump V is connected with a liquid inlet end of the rotary evaporator II through a pipeline. According to the method, high additional organic matters in the tar residues can be effectively extracted by adopting a mode of synergism of ultrasonic-assisted extraction and column chromatography separation, so that resource utilization of the tar residues is realized. The solvent and the eluent selected in the whole process can be recycled through a rotary evaporator, the operation cost is low, and near-zero emission can be realized.

Description

Technical Field

[0001] The utility model relates to the field of tar residue separation and conversion, in particular to a system for step-by-step separation and conversion of tar residue. Background Art

[0002] Tar residue is a toxic, hazardous, and viscous solid waste produced as a byproduct of coal coking or gasification. Tar residue contains a large amount of polycyclic aromatic compounds (PACs) known to be carcinogenic, teratogenic, and mutagenic. Direct incineration releases these toxic substances, resulting in adverse effects on humans and the environment. Currently, resource utilization of tar residue in my country primarily involves coking with coal and preparing activated carbon. However, these methods significantly waste the abundant PACs present in tar residue, particularly the condensed aromatic compounds that are difficult to synthesize artificially, which remain unisolated and unutilized. Utility Model Content

[0003] In response to the above-mentioned deficiencies in the prior art, the utility model provides a system for the step-by-step separation and conversion of tar residue. By developing a suitable process, high-value-added organic matter in tar residue is selectively extracted to achieve the purpose of separating aromatic chemicals from tar residue, thereby achieving high-value utilization of tar residue.

[0004] In order to achieve the above-mentioned purpose of the invention, the technical solution adopted by the present utility model is:

[0005] Provided is a system for stepwise separation and conversion of tar residue, comprising an ultrasonic cleaner, wherein a liquid outlet of the ultrasonic cleaner is connected to a solid-liquid separator via a pipeline, a liquid outlet of an upper liquid layer of the solid-liquid separator is connected to a delivery pump I via a pipeline, the delivery pump I is connected to a liquid inlet of a rotary evaporator I via a pipeline, concentrated organic matter in the rotary evaporator I is connected to an upper end of a vertically arranged chromatography column via a pipeline, the lower end of the chromatography column is connected to a sand core funnel, a collecting tank is placed below the outlet of the sand core funnel, the collecting tank is connected to a delivery pump V via a pipeline, and the delivery pump V is connected to a liquid inlet of the rotary evaporator II via a pipeline.

[0006] Furthermore, the bottom of the solid-liquid separator is connected to the delivery pump II through a pipeline, the delivery pump II is connected to the upper feed port of the high-temperature reactor through a pipeline, the lower collecting port of the rotary evaporator I is connected to the upper feed port of the high-temperature reactor through a pipeline, the discharge port of the high-temperature reactor is connected to the collecting tank I through a pipeline, and the lower end of the collecting tank I is connected to the feed end of the ultrasonic cleaner through a pipeline and the delivery pump III.

[0007] Furthermore, the chromatography column includes two chromatography columns I and chromatography column II connected in series, and the chromatography columns I and chromatography columns II are both arranged vertically. The lower ends of the chromatography columns I and chromatography columns II are respectively provided with sand core funnels I and sand core funnels II, and the lower ends of the sand core funnels I and sand core funnels II are respectively placed with collection tanks II and collection tanks III. The collection tank II is connected to the upper end of the chromatography column II through a pipeline and a delivery pump IV, and the collection tank III is connected to the rotary evaporator II through a delivery pump V. The concentrated organic matter in the rotary evaporator I is transported to the chromatography column I through a pipeline.

[0008] Furthermore, the lower ends of the sand core funnel I and the sand core funnel II are both provided with flow regulating valves.

[0009] Furthermore, the chromatography column I is a forward chromatography column, and the chromatography column II is a reverse chromatography column.

[0010] The beneficial effects of the utility model are:

[0011] 1. The utility model adopts the method of ultrasonic-assisted extraction and column chromatography separation to effectively extract high-added organic matter in tar residue, thereby realizing the resource utilization of tar residue.

[0012] 2. The utility model adopts a separation method combining forward and reverse chromatographic column chromatography to effectively extract high value-added organic matter from tar residue.

[0013] 3. The solvents and eluents used in the processes executed by the entire process system can be recycled through the rotary evaporator, with low operating costs and near-zero emissions. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 Schematic diagram of the system for the step-by-step separation and conversion of tar residue.

[0015] Figure 2 Flow chart of the step-by-step separation and conversion method of tar residue.

[0016] Among them, 1. Ultrasonic cleaning instrument, 2. Solid-liquid separator, 3. Delivery pump I, 4. Delivery pump II, 5. Collection tank I, 6. Delivery pump III, 7. Rotary evaporator I, 8. High-temperature reactor, 9. Chromatography column I, 10. Sand core funnel I, 11. Flow regulating valve, 12. Collection tank II, 13. Delivery pump IV, 14. Chromatography column II, 15. Sand core funnel II, 16. Collection tank III, 17. Delivery pump V, 18. Rotary evaporator II. DETAILED DESCRIPTION

[0017] The specific implementation methods of the present invention are described below to facilitate understanding of the present invention by those skilled in the art. However, it should be clear that the present invention is not limited to the scope of the specific implementation methods. For those skilled in the art, as long as various changes are within the spirit and scope of the present invention as defined and determined by the appended claims, these changes are obvious, and all utility model creations using the concept of the present invention are protected.

[0018] like Figure 1 As shown, a system for stepwise separation and conversion of tar residue includes an ultrasonic cleaner 1, the liquid outlet of the ultrasonic cleaner 1 is connected to a solid-liquid separator 2 through a pipeline, the liquid outlet of the upper liquid layer of the solid-liquid separator 2 is connected to a delivery pump I3 through a pipeline, the delivery pump I3 is connected to the liquid inlet of a rotary evaporator I7 through a pipeline, the concentrated organic matter in the rotary evaporator I7 is transported to a vertically arranged chromatography column through a pipeline, the lower end of the chromatography column is connected to a sand core funnel, a collecting tank is placed below the outlet of the sand core funnel, the collecting tank is connected to the rotary evaporator II18 through a delivery pump V17, and the delivery pump V17 is connected to the liquid inlet of the rotary evaporator II18 through a pipeline.

[0019] This solution uses ultrasonic dissolution of the ultrasonic cleaning apparatus 1 to improve the efficiency of tar residue extraction. The tar residue is extracted in the ultrasonic cleaning apparatus 1 at a frequency of 100 KHz at room temperature for 30 minutes.

[0020] In this embodiment, the bottom of solid-liquid separator 2 is connected to delivery pump II4 via a pipeline, which is connected to the upper feed port of high-temperature reactor 8 via a pipeline. The lower collection port of rotary evaporator I7 is connected to the upper feed port of high-temperature reactor 8 via a pipeline. The discharge port of high-temperature reactor 8 is connected to collection tank I5 via a pipeline. The lower end of collection tank I5 is connected to the feed port of ultrasonic cleaning apparatus 1 via a pipeline and delivery pump III6. The solvent in the extract is extracted and recovered by solid-liquid separator 2 and high-temperature reactor 8, achieving solvent recycling.

[0021] In this embodiment, the chromatography column includes two chromatography columns connected in series, chromatography columns I9 and chromatography columns II14. Both chromatography columns I9 and chromatography columns II14 are arranged vertically. Sand core funnels I10 and II15 are respectively provided at the lower ends of chromatography columns I9 and chromatography columns II14. Collection tanks II12 and III16 are respectively placed below sand core funnels I10 and II15. Collection tank II12 is connected to the upper end of chromatography column II14 via a pipeline and a delivery pump IV13. Collection tank III16 is connected to a delivery pump V17 via a pipeline. The concentrated organic matter in rotary evaporator I7 is transported to chromatography column I9 via a pipeline. Chromatography column I9 is a forward chromatography column, and chromatography column II14 is a reverse chromatography column. Gradual elution is performed through the two chromatography columns, and the eluate at each stage is controlled by a flow control valve 11 and enriched in the collection tank.

[0022] In this embodiment, the lower ends of the sand core funnel I 10 and the sand core funnel II 15 are both provided with flow regulating valves 11 for regulating. During the graded elution process, the flow regulating valves 11 can control the elution process and achieve separation of the eluates at each level.

[0023] like Figure 2 As shown, a method for stepwise separation and conversion of tar residue using the above-mentioned system for stepwise separation and conversion of tar residue comprises the following steps:

[0024] S1: Mix tar residue and petroleum ether at a ratio of 1 g:8 ml, add the mixture to an ultrasonic cleaner 1 and extract at a temperature of 20-40°C for 30 minutes. Add the extracted mixture to a solid-liquid separator 2 for solid-liquid separation to obtain an upper layer of extract and a lower layer of raffinate, and ensure that the upper layer of extract is colorless;

[0025] S2: The upper layer of the extract is pumped into a rotary evaporator I7 via a delivery pump I3, and the lower layer of the extract residue is pumped into a high-temperature reactor 8 via a delivery pump II4. The upper layer of the extract is heated and distilled in the rotary evaporator I7, condensed and recovered into petroleum ether, which is then discharged into the high-temperature reactor 8 and distilled and separated to obtain a preliminary enrichment in the tar residue;

[0026] S3: The recovered petroleum ether and the extract residue are thermally dissolved in a high-temperature reactor 8 at 90°C; at the same time, methanol, CS2, acetone, and an equal volume of a mixture of acetone and CS2 are sequentially added to the high-temperature reactor 8, and the hot-soluble residue is fully extracted at 65, 57, 47, and 60°C in sequence to obtain a hot-soluble extract, which is discharged into a collection tank I5;

[0027] S4: The delivery pump III 6 extracts the hot-melt extract from the collection tank I 5 and discharges it into the ultrasonic cleaning apparatus 1 , thereby realizing repeated recycling of the solvent in the high-temperature reactor 8 ;

[0028] S5: Weigh an appropriate amount of silica gel, discharge the preliminary enrichment in the tar residue into the forward chromatographic column, and then fill the silica gel into the forward chromatographic column. After that, add eluents to the forward chromatographic column in the following order: petroleum ether, a mixture of petroleum ether and ethyl acetate in a ratio of 4ml:1ml, a mixture of ethyl acetate and methanol in a ratio of 4ml:1ml, a mixture of ethyl acetate and methanol in a ratio of 1ml:1ml, and a mixture of ethyl acetate and methanol in a ratio of 1ml:4ml. The eluents are used as the mobile phase for gradient elution;

[0029] S6: After the gradient elution, the eluates of each level are sequentially enriched in the collection tank II 12. The eluates of each level obtained by the gradient elution are controlled by the flow control valve 11. Each time an eluent is added, an eluate is obtained. Afterwards, the eluates of each level obtained by the gradient elution are sequentially input into the reverse phase chromatography column through the delivery pump IV 13.

[0030] S7: Octadecyl bonded silica gel is used as the filler in the reverse phase chromatography column, and the same eluent as in the forward chromatography column is added in sequence for gradient elution and reverse elution. The eluate obtained by the reverse elution is enriched in the collection tank III16, and then transported to the rotary evaporator II18 for evaporation and concentration through the delivery pump V17.

[0031] This utility model utilizes ultrasound-assisted extraction and column chromatography separation to effectively extract high-value organic matter from tar residue, thereby realizing resource utilization of tar residue. This utility model utilizes a combination of forward and reverse column chromatography to effectively extract high-value organic matter from tar residue. The solvents and eluents used in the entire process can be recycled using a rotary evaporator, resulting in low operating costs and near-zero emissions.

Claims

1. A system for the step-by-step separation and conversion of tar residues, characterized in that: The invention comprises an ultrasonic cleaning instrument, wherein the liquid outlet end of the ultrasonic cleaning instrument is connected to a solid-liquid separator through a pipeline, the liquid outlet end of the upper liquid layer of the solid-liquid separator is connected to a delivery pump I through a pipeline, the delivery pump I is connected to the liquid inlet end of a rotary evaporator I through a pipeline, the concentrated organic matter in the rotary evaporator I is transported to a vertically arranged chromatography column through the pipeline, the lower end of the chromatography column is connected to a sand core funnel, a collecting tank is placed below the outlet of the sand core funnel, the collecting tank is connected to a delivery pump V through a pipeline, and the delivery pump V is connected to the liquid inlet end of the rotary evaporator II through a pipeline.

2. The system for stepwise separation and conversion of tar residue according to claim 1, characterized in that: The bottom of the solid-liquid separator is connected to the delivery pump II through a pipeline, the delivery pump II is connected to the upper feed port of the high-temperature reactor through a pipeline, the lower collection port of the rotary evaporator I is connected to the upper feed port of the high-temperature reactor through a pipeline, the discharge port of the high-temperature reactor is connected to the collection tank I through a pipeline, and the lower end of the collection tank I is connected to the feed end of the ultrasonic cleaner through a pipeline and the delivery pump III.

3. The system for stepwise separation and conversion of tar residue according to claim 1, characterized in that: The chromatography column includes two chromatography columns I and II connected in series, and the chromatography columns I and II are both arranged vertically. Sand core funnels I and II are respectively provided at the lower ends of the chromatography columns I and II. Collection tanks II and III are respectively placed below the sand core funnels I and II. The collection tank II is connected to the upper end of the chromatography column II through a pipeline and a delivery pump IV. The collection tank III is connected to the rotary evaporator II through a delivery pump V. The concentrated organic matter in the rotary evaporator I is transported to the chromatography column I through a pipeline.

4. The system for stepwise separation and conversion of tar residue according to claim 3, characterized in that: The lower ends of the sand core funnel I and the sand core funnel II are both provided with flow regulating valves.

5. The system for stepwise separation and conversion of tar residue according to claim 3, characterized in that: The chromatography column I is a forward chromatography column, and the chromatography column II is a reverse chromatography column.

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