CN112500884A - Method for removing sulfide in solvent oil - Google Patents
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- CN112500884A CN112500884A CN202011239006.6A CN202011239006A CN112500884A CN 112500884 A CN112500884 A CN 112500884A CN 202011239006 A CN202011239006 A CN 202011239006A CN 112500884 A CN112500884 A CN 112500884A
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- 239000002904 solvent Substances 0.000 title claims abstract description 132
- 238000000034 method Methods 0.000 title claims abstract description 37
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims description 11
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 136
- 230000023556 desulfurization Effects 0.000 claims abstract description 136
- 238000000605 extraction Methods 0.000 claims abstract description 63
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000012546 transfer Methods 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 5
- 150000003568 thioethers Chemical class 0.000 claims abstract 11
- 230000008929 regeneration Effects 0.000 claims description 16
- 238000011069 regeneration method Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims 3
- 239000011707 mineral Substances 0.000 claims 3
- 235000015096 spirit Nutrition 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 description 54
- 229910052717 sulfur Inorganic materials 0.000 description 54
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 51
- 239000007788 liquid Substances 0.000 description 15
- 238000004064 recycling Methods 0.000 description 15
- 238000000926 separation method Methods 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000005804 alkylation reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002795 fluorescence method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 102100034544 Acyl-CoA 6-desaturase Human genes 0.000 description 1
- 101000737578 Arabidopsis thaliana Bifunctional cystathionine gamma-lyase/cysteine synthase Proteins 0.000 description 1
- 101000848255 Homo sapiens Acyl-CoA 6-desaturase Proteins 0.000 description 1
- 101000952234 Homo sapiens Sphingolipid delta(4)-desaturase DES1 Proteins 0.000 description 1
- 101000918926 Homo sapiens Sphingolipid delta(4)-desaturase/C4-monooxygenase DES2 Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 101100330363 Physcomitrium patens DES5 gene Proteins 0.000 description 1
- 101100277598 Sorghum bicolor DES3 gene Proteins 0.000 description 1
- 102100037416 Sphingolipid delta(4)-desaturase DES1 Human genes 0.000 description 1
- 102100029473 Sphingolipid delta(4)-desaturase/C4-monooxygenase DES2 Human genes 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000001741 organic sulfur group Chemical group 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 229910052815 sulfur oxide Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method for removing sulfides in solvent oil, which comprises the following steps of multi-stage cross-flow extraction desulfurization: mixing the solvent oil and the desulfurization solvent, stirring, standing and layering in a separating funnel to obtain an upper raffinate oil phase and a lower desulfurization solvent phase, and extracting and then taking the upper raffinate oil phase for repeated operation; or multi-stage countercurrent extraction desulfurization: the desulfurization solvent and the solvent oil are respectively sprayed into the tower top and the tower bottom of the packed tower, the desulfurization solvent phase is used as a dispersion phase, the solvent oil flows out of the tower from the top to the bottom, the desulfurization solvent is contacted with the solvent oil from the top to the bottom, and the mass transfer is carried out, and the desulfurization solvent is discharged from the tower bottom. The method for multi-stage cross-flow extraction desulfurization or multi-stage countercurrent extraction has the advantages that the extraction desulfurization rates can reach 99.80 percent and 92.49 percent respectively, and the process adopts continuous operation, so that the green production process is realized.
Description
Technical Field
The invention relates to a desulfurization method, in particular to a method for removing sulfide in solvent oil.
Background
Due to environmental concerns, strict regulations have been imposed on the sulfur content of petroleum products in countries over the last few decades. The sulfur oxides released from the oil contaminated with organic sulfur will acidify the water source and soil through acid rain, thus causing irreparable damage to the ecosystem. In addition, the solvent oil product in China has the disadvantages of higher sulfur content and aromatic hydrocarbon content compared with the solvent oil product in foreign countries. Therefore, it is important to remove sulfur compounds from the miscella.
Currently the most widely used industryThe desulfurization technique is hydrodesulfurization, in which sulfur-containing substances in raw materials are reacted with hydrogen at the active center of a catalyst under the adsorption action of a high-activity catalyst to generate H under the conditions of high temperature and high pressure2S gas, thereby removing it. Although the hydrodesulfurization technology has strong processing capacity and high desulfurization efficiency, the device cost and energy consumption are relatively high, and the device is difficult to be suitable for some small and medium-sized enterprises. Adsorptive desulfurization techniques are also well established in industry and are generally used to remove sulfur-containing components by chemically bonding together the active components on the adsorbent by van der waals forces or by chemical reaction. The method has strong adsorption force and high selectivity, but the method has small adsorption capacity and large dosage of required adsorbent, thereby resulting in higher cost. The alkylation desulfurization technology also has a mature process in industry, and generally increases the boiling point of sulfide through alkylation reaction under the action of a catalyst, so that the sulfide is separated through rectification. But the large-scale application of the catalyst is limited by the disadvantages of side reaction in the reaction, easy corrosion of equipment, environmental pollution, high requirement on the catalyst and the like.
Besides, the method of oxidative desulfurization, biological desulfurization, extraction desulfurization and the like in a laboratory can also remove the sulfide in the oil product. Wherein, the operation condition of the extraction desulfurization technology is simple and mild, and the quality of the obtained oil product is not influenced. Such as acid-base refining desulfurization process still used in industry. However, the efficiency of the existing extraction desulfurization method is still not ideal.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a method for removing sulfides in solvent naphtha, which can be operated continuously and has high efficiency.
The technical scheme is as follows: the method for removing the sulfide in the solvent oil comprises the following steps:
multi-stage cross-flow extraction desulfurization: mixing the solvent oil and the desulfurization solvent, stirring, standing and layering in a separating funnel to obtain an upper raffinate oil phase and a lower desulfurization solvent phase, and extracting and then taking the upper raffinate oil phase for repeated operation;
or multi-stage countercurrent extraction desulfurization: the desulfurization solvent and the solvent oil are respectively sprayed into the tower top and the tower bottom of the packed tower, the desulfurization solvent phase is used as a dispersion phase, the solvent oil flows out of the tower from the top to the bottom, the desulfurization solvent is contacted with the solvent oil from the top to the bottom, and the mass transfer is carried out, and the desulfurization solvent is discharged from the tower bottom.
Preferably, the desulfurization solvent after the multi-stage cross-flow extraction desulfurization or the multi-stage countercurrent extraction desulfurization extraction can be regenerated.
Preferably, the regeneration process is: and adding water into the lower-layer desulfurization solvent phase, mixing and stirring to separate out and filter sulfide, and distilling and drying the obtained desulfurization solvent phase to obtain the regenerated desulfurization solvent.
Preferably, in the regeneration process of the desulfurization solvent, the molar ratio of water to the desulfurization solvent phase is 0.5-2: 1; the stirring time is 120-180 min.
Preferably, in the multi-stage cross-flow extraction desulfurization or multi-stage countercurrent extraction desulfurization process, the mass ratio of the solvent oil to the desulfurization solvent is 0.5-2: 1.
Preferably, multi-stage cross-flow extraction desulfurization is included: mixing the solvent oil and the desulfurization solvent, stirring, standing and layering in a separating funnel to obtain an upper raffinate oil phase and a lower desulfurization solvent phase, and extracting and then taking the upper raffinate oil phase for repeated operation; the stirring temperature of the extraction is 10-35 ℃, and the stirring speed is 500-1000 rpm.
Preferably, multi-stage cross-flow extraction desulfurization is included: mixing the solvent oil and the desulfurization solvent, stirring, standing and layering in a separating funnel to obtain an upper raffinate oil phase and a lower desulfurization solvent phase, and extracting and then taking the upper raffinate oil phase for repeated operation; the stirring time is 60-120 min, and the standing time is 5-30 min.
Preferably, multi-stage countercurrent extraction desulfurization is included: spraying a desulfurization solvent and solvent oil from the top and the bottom of a packed tower respectively, taking a desulfurization solvent phase as a dispersion phase, enabling the solvent oil to flow out of the tower from the top to the bottom, enabling the desulfurization solvent to contact and transfer mass with the solvent oil from the top to the bottom, and discharging the mass to the bottom of the tower; the temperature in the packed tower is 10-35 ℃; the extraction stage number of the multi-stage countercurrent extraction process is 1-3 stages.
Preferably, the method comprises multi-stage cross-flow extraction desulfurization, wherein the number of extraction stages is 1-6.
Preferably, the boiling range of the solvent oil is 130-190 ℃, and the density of the solvent oil is 0.70-0.80 g/cm3(ii) a The sulfur content is 16000 ppm-20000 ppm.
Has the advantages that: compared with the prior art, the invention has the following remarkable effects: 1. continuous operation is adopted, multi-stage cross-flow extraction desulfurization operation is carried out on the high-sulfur alkane solvent oil, the single-stage extraction desulfurization rate is 62.00 percent, and the sulfur content is reduced to 6819 ppm; the 6-stage extraction desulfurization rate is 99.80 percent, and the sulfur content is reduced to 36 ppm; and the multi-stage countercurrent extraction desulfurization operation is carried out on the low-sulfur alkane solvent oil, the 3-stage extraction desulfurization rate is 92.49%, and the sulfur content is reduced to 66 ppm. 2. After the extracted desulfurization solvent is subjected to back extraction and regeneration, the high-sulfur alkane solvent oil is subjected to single-stage extraction and desulfurization operation under the same condition, and after 5 times of circulating regeneration, the desulfurization rate is 58.65%, and the desulfurization rate is not remarkably reduced compared with that of a fresh desulfurization solvent.
Detailed Description
The present invention is described in further detail below.
Example 1
The desulfurization solvent used in the process of the present invention may be a commonly commercially available desulfurization solvent, and it is preferable to use a eutectic solvent. Adding a desulfurization solvent and sulfur-containing solvent oil with the sulfur content of 17945ppm into a flask according to the mass ratio of 0.5:1, stirring for 120min at 25 ℃ and normal pressure at the stirring speed of 1000rpm, standing for 15min, and then layering; and taking the lower-layer desulfurization solvent phase after liquid separation, and recycling the lower-layer desulfurization solvent phase through regeneration operation for recycling.
The invention adopts an ultraviolet fluorescence method specified in SH/T0689-. Wherein the detection range of the ultraviolet fluorescence method is 1-8000 ppm. As shown in figure 1, a sulfur measurement test device takes 1.5-3 mL of a sample to be measured and puts the sample into a combustion bottle for combustion, a pump is started to enable generated sulfur dioxide to uniformly and gently enter an absorber through a flue and be absorbed by a sodium carbonate aqueous solution in the absorber, then 0.05mol/L hydrochloric acid solution is used for titrating an absorption solution, and the sulfur content is measured by a volumetric analysis method.
The desulfurization rate calculation formula is as follows:
wherein eta is the desulfurization rate, c0As initial sulfur content, ctIs the residual sulfur content after desulfurization.
In the embodiment, the upper oil phase is taken to analyze the sulfur content, and the result shows that the sulfur content is reduced to 9349ppm after DES1 is added for extraction, and the desulfurization rate is 47.90% through calculation; after DES2 is added for extraction, the sulfur content is reduced to 8916ppm, and the desulfurization rate is 50.31%; after DES3 is added, the sulfur content is reduced to 9220ppm, and the desulfurization rate is 48.62%.
Example 2
Adding a desulfurization solvent and sulfur-containing solvent oil with the sulfur content of 17945ppm into a flask according to the mass ratio of 1:1, stirring for 120min at 25 ℃ and normal pressure at the stirring speed of 1000rpm, standing for 15min, and then layering; taking the lower layer of the desulfurization solvent phase after liquid separation, and recycling the lower layer of the desulfurization solvent phase through regeneration operation for recycling;
the upper oil phase is taken to analyze the sulfur content, and the result shows that the sulfur content is reduced to 6819ppm after the DES4 is added for extraction, and the desulfurization rate is 62.00 percent; after DES5 was added, the sulfur content was reduced to 6979ppm, the desulfurization rate was 61.11%, and after DES6 was added, the sulfur content was reduced to 7104ppm, the desulfurization rate was 60.41%.
Example 3
Adding a desulfurization solvent and sulfur-containing solvent oil with the sulfur content of 17945ppm into a flask according to the mass ratio of 2:1, stirring for 120min at the temperature of 25 ℃ and under normal pressure, stirring at the speed of 1000rpm, and standing for 15min to perform 2-level cross-flow extraction operation; taking the lower layer of the desulfurization solvent phase after liquid separation, and recycling the lower layer of the desulfurization solvent phase through regeneration operation for recycling; the upper oil phase was taken for analysis of the sulfur content, which showed that the sulfur content was reduced to 1945ppm, which was calculated to give a desulfurization rate of 89.16%.
Example 4
Adding a desulfurization solvent and sulfur-containing solvent oil with the sulfur content of 17945ppm into a flask according to the mass ratio of 1:1, stirring for 120min at 25 ℃ and normal pressure, stirring at the speed of 1000rpm, and standing for 15min to perform 3-level cross-flow extraction operation. Taking the lower layer of the desulfurization solvent phase after liquid separation, and recycling the lower layer of the desulfurization solvent phase through regeneration operation for recycling; the upper oil phase was taken for analysis of sulfur content, and the results showed that sulfur content was reduced to 879ppm, which was calculated to give a desulfurization rate of 95.10%.
Example 5
Adding a desulfurization solvent and sulfur-containing solvent oil with the sulfur content of 17945ppm into a flask according to the mass ratio of 1:1, stirring for 120min at 25 ℃ and normal pressure, stirring at the speed of 1000rpm, and standing for 15min to perform 6-stage cross-flow extraction operation. Taking the lower layer of the desulfurization solvent phase after liquid separation, and recycling the lower layer of the desulfurization solvent phase through regeneration operation for recycling; the upper oil phase is taken to analyze the sulfur content, and the result shows that the sulfur content is reduced to 36ppm, and the desulfurization rate is calculated to be 99.80 percent.
Example 6
Adding a desulfurization solvent from the top of a packed extraction tower at the speed of 1.68L/h, feeding sulfur-containing solvent oil with the sulfur content of 879ppm from the bottom of the packed extraction tower at the speed of 0.84L/h through a sprayer, keeping the temperature in the tower at 25 ℃, setting the theoretical stage number of the packed extraction tower at 1 stage, and respectively flowing out from the top and the bottom of the tower after two phases are contacted and transferred in the tower. Taking the heavy liquid layer at the bottom of the tower, and recycling the heavy liquid layer through regeneration operation for reuse; and (3) taking the supernatant liquid at the top of the tower for analyzing the sulfur content, wherein the result shows that the sulfur content is reduced to 284ppm, and the desulfurization rate is 67.69% by calculation.
Example 7
Adding a desulfurization solvent from the top of a packed extraction tower at the speed of 0.42L/h, feeding sulfur-containing solvent oil with the sulfur content of 879ppm from the bottom of the packed extraction tower at the speed of 0.84L/h through a sprayer, keeping the temperature in the tower at 25 ℃, wherein the theoretical stage number of the packed extraction tower is 2, and the two phases flow out from the top and the bottom of the tower respectively after being contacted and subjected to mass transfer in the tower. Taking the heavy liquid layer at the bottom of the tower, and recycling the heavy liquid layer through regeneration operation for reuse; and (3) taking a supernatant liquid at the top of the tower for analyzing the sulfur content, wherein the result shows that the sulfur content is reduced to 249ppm, and the desulfurization rate is calculated to be 71.67%.
Example 8
Adding a desulfurization solvent from the top of a packed extraction tower at the speed of 0.84L/h, feeding sulfur-containing solvent oil with the sulfur content of 879ppm from the bottom of the packed extraction tower at the speed of 0.84L/h through a sprayer, keeping the temperature in the tower at 25 ℃, and the theoretical stage number of the packed extraction tower at 3 stages, wherein two phases are contacted and subjected to mass transfer in the tower and then respectively flow out from the top and the bottom of the tower. Taking the heavy liquid layer at the bottom of the tower, and recycling the heavy liquid layer through regeneration operation for reuse; and (3) taking the supernatant liquid at the top of the tower for analyzing the sulfur content, wherein the result shows that the sulfur content is reduced to 66ppm, and the desulfurization rate is 92.49% by calculation.
Example 9
The basic extraction procedure is the same as example 1, except that the lower layer of the desulfurized solvent phase after extraction is taken and added with water with the molar ratio of 0.5 time to 2 times respectively, the mixture is stirred for 120min and then kept stand for 12h, sulfide is separated out and then filtered and removed, a rotary evaporator is added to remove excessive moisture, and the regenerated desulfurized solvent is obtained after vacuum drying respectively.
Example 10
The basic extraction procedure was the same as in example 1, except that the lower desulfurization solvent phase after extraction was taken and added with water in a molar ratio of 1 time, stirred for 120min and then allowed to stand for 12h, after separation of the sulfide, it was filtered off and then added to a rotary evaporator to remove excess water, and the regenerated desulfurization solvent was obtained after vacuum drying.
The desulfurization solvent used in examples 3 to 8 was regenerated 1 to 5 times and added to a flask in a mass ratio of 1:1 with sulfur-containing solvent naphtha having a sulfur content of 17945ppm, and the mixture was stirred at 25 ℃ and atmospheric pressure for 120 minutes at a stirring speed of 1000rpm, left to stand for 15 minutes, and then layered. Taking the lower layer of the desulfurization solvent phase after liquid separation, and recycling the lower layer of the desulfurization solvent phase through regeneration operation for recycling; the oil phase was removed and analyzed for sulfur content and the results are shown in Table 1.
TABLE 1 regenerated DES desulfurization performance
As can be seen from Table 1, the DES desulfurization performance is not significantly reduced after 5 regenerations, which indicates that the desulfurization solvent has good regenerability and can be recycled.
The cases show that the extraction desulfurization step provided by the invention is simple to operate, has low cost and no pollution to the environment, can be used for deep desulfurization of solvent oil, and can be recycled.
Claims (10)
1. A method for removing sulfides in solvent oil is characterized by comprising the following steps:
multi-stage cross-flow extraction desulfurization: mixing the solvent oil and the desulfurization solvent, stirring, standing and layering in a separating funnel to obtain an upper raffinate oil phase and a lower desulfurization solvent phase, and extracting and then taking the upper raffinate oil phase for repeated operation;
or multi-stage countercurrent extraction desulfurization: the desulfurization solvent and the solvent oil are respectively sprayed into the tower top and the tower bottom of the packed tower, the desulfurization solvent phase is used as a dispersion phase, the solvent oil flows out of the tower from the top to the bottom, the desulfurization solvent is contacted with the solvent oil from the top to the bottom, and the mass transfer is carried out, and the desulfurization solvent is discharged from the tower bottom.
2. The method for removing sulfides from solvent oil according to claim 1, wherein the desulfurization solvent after the multi-stage cross-flow extraction desulfurization or multi-stage counter-current extraction desulfurization extraction is renewable.
3. The method for removing sulfides from solvent oil according to claim 2, wherein the regeneration process is: and adding water into the lower-layer desulfurization solvent phase, mixing and stirring to separate out and filter sulfide, and distilling and drying the obtained desulfurization solvent phase to obtain the regenerated desulfurization solvent.
4. The method for removing sulfides in mineral spirits according to claim 3, wherein the molar ratio of water to the desulfurization solvent phase during the regeneration of the desulfurization solvent is 0.5-2: 1.
5. The method for removing sulfides in the solvent oil according to claim 1, wherein the mass ratio of the solvent oil to the desulfurization solvent in the multi-stage cross-flow extraction desulfurization or multi-stage counter-current extraction desulfurization process is 0.5-2: 1.
6. The method for removing sulfides from solvent oil according to claim 1, comprising multi-stage cross-flow extraction desulfurization: mixing the solvent oil and the desulfurization solvent, stirring, standing and layering in a separating funnel to obtain an upper raffinate oil phase and a lower desulfurization solvent phase, and extracting and then taking the upper raffinate oil phase for repeated operation; the stirring temperature of the extraction is 10-35 ℃, and the stirring speed is 500-1000 rpm.
7. The method for removing sulfides from solvent oil according to claim 1, comprising multi-stage cross-flow extraction desulfurization: mixing the solvent oil and the desulfurization solvent, stirring, standing and layering in a separating funnel to obtain an upper raffinate oil phase and a lower desulfurization solvent phase, and extracting and then taking the upper raffinate oil phase for repeated operation; the stirring time is 60-120 min, and the standing time is 5-30 min.
8. The method for removing sulfides from solvent oil according to claim 1, comprising multi-stage countercurrent extraction desulfurization: spraying a desulfurization solvent and solvent oil from the top and the bottom of a packed tower respectively, taking a desulfurization solvent phase as a dispersion phase, enabling the solvent oil to flow out of the tower from the top to the bottom, enabling the desulfurization solvent to contact and transfer mass with the solvent oil from the top to the bottom, and discharging the mass to the bottom of the tower; the temperature in the packed tower is 10-35 ℃.
9. The method for removing sulfides in the solvent oil according to claim 1, comprising multi-stage cross-flow extraction desulfurization, wherein the number of extraction stages is 1-6.
10. The method for removing sulfides from the mineral spirit according to claim 1, wherein the mineral spirit has a boiling range of 130 to 190 ℃ and a density of 0.70 to 0.80g/cm3。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104762100A (en) * | 2015-03-30 | 2015-07-08 | 浙江大学 | Method for removing nitrogen-containing compounds in oil products by virtue of eutectic solvent extraction |
| CN108192655A (en) * | 2018-01-24 | 2018-06-22 | 中国石油大学(华东) | A kind of method for extracting removing Sulfur Compounds from Crude Oils |
| CN108893137A (en) * | 2018-07-18 | 2018-11-27 | 华东理工大学 | A kind of water base eutectic solvent and preparation method thereof and a kind of oil product extraction desulphurization method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104762100A (en) * | 2015-03-30 | 2015-07-08 | 浙江大学 | Method for removing nitrogen-containing compounds in oil products by virtue of eutectic solvent extraction |
| CN108192655A (en) * | 2018-01-24 | 2018-06-22 | 中国石油大学(华东) | A kind of method for extracting removing Sulfur Compounds from Crude Oils |
| CN108893137A (en) * | 2018-07-18 | 2018-11-27 | 华东理工大学 | A kind of water base eutectic solvent and preparation method thereof and a kind of oil product extraction desulphurization method |
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