JP5824137B2 - 硫化ナトリウムの分離及び精製方法 - Google Patents
硫化ナトリウムの分離及び精製方法 Download PDFInfo
- Publication number
- JP5824137B2 JP5824137B2 JP2014504453A JP2014504453A JP5824137B2 JP 5824137 B2 JP5824137 B2 JP 5824137B2 JP 2014504453 A JP2014504453 A JP 2014504453A JP 2014504453 A JP2014504453 A JP 2014504453A JP 5824137 B2 JP5824137 B2 JP 5824137B2
- Authority
- JP
- Japan
- Prior art keywords
- solution
- organic solvent
- water
- sludge
- desulfurization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000034 method Methods 0.000 title claims description 77
- 238000000746 purification Methods 0.000 title claims description 16
- 229910052979 sodium sulfide Inorganic materials 0.000 title description 25
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 title description 25
- 238000000926 separation method Methods 0.000 title description 13
- 239000011734 sodium Substances 0.000 claims description 78
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 45
- 239000008096 xylene Substances 0.000 claims description 45
- 238000006477 desulfuration reaction Methods 0.000 claims description 41
- 230000023556 desulfurization Effects 0.000 claims description 41
- 239000010802 sludge Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000003960 organic solvent Substances 0.000 claims description 35
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 34
- 239000003208 petroleum Substances 0.000 claims description 33
- 239000000203 mixture Substances 0.000 claims description 28
- 235000010265 sodium sulphite Nutrition 0.000 claims description 17
- 239000008346 aqueous phase Substances 0.000 claims description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 13
- 229930195733 hydrocarbon Natural products 0.000 claims description 11
- 150000002430 hydrocarbons Chemical class 0.000 claims description 11
- 239000004215 Carbon black (E152) Substances 0.000 claims description 10
- 239000012074 organic phase Substances 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 7
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 6
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N methylene hexane Natural products CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000002955 isolation Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 150000001345 alkine derivatives Chemical class 0.000 claims description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 3
- -1 cyclic alkenes Chemical class 0.000 claims description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000010926 purge Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 37
- 239000003921 oil Substances 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 14
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 13
- 239000006227 byproduct Substances 0.000 description 13
- 229910052708 sodium Inorganic materials 0.000 description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000010779 crude oil Substances 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 150000002898 organic sulfur compounds Chemical class 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 239000000295 fuel oil Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 150000003464 sulfur compounds Chemical class 0.000 description 3
- MARCAKLHFUYDJE-UHFFFAOYSA-N 1,2-xylene;hydrate Chemical compound O.CC1=CC=CC=C1C MARCAKLHFUYDJE-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003738 xylenes Chemical class 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005457 optimization 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
- 238000005504 petroleum refining Methods 0.000 description 1
- 238000011175 product filtration Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/14—Preparation of sulfites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/80—Destroying solid waste or transforming solid waste into something useful or harmless involving an extraction step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/36—Purification
-
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
-
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
-
- 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
- C10G21/06—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents characterised by the solvent used
- C10G21/12—Organic compounds only
- C10G21/14—Hydrocarbons
-
- 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
- C10G29/00—Refining of hydrocarbon oils, in the absence of hydrogen, with other chemicals
- C10G29/04—Metals, or metals deposited on a carrier
-
- 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
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/08—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one sorption step
-
- 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
- C10G7/00—Distillation of hydrocarbon oils
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1077—Vacuum residues
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Treatment Of Sludge (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Description
本開示の目的は、石油残渣の脱硫の際に形成された硫化ナトリウム(Na2S)の単離及び精製のためのプロセスを提供することである。
本開示の別の目的は、石油残渣の脱硫の際に形成されたNa2Sから亜硫酸ナトリウム(Na2SO3)を得るためのプロセスを提供することである。
−少なくとも1種の有機溶媒と水との混合物を調製する工程と;
−混合物を約25〜100℃の温度で約20分〜2時間にわたって撹拌しながらスラッジに添加し、場合により冷却して溶液を得る工程と;
−溶液を分離漏斗に移して静置させ、Na2Sを含有する水相と石油を含有する有機相との混合物を得る工程と;
−2相のそれぞれを別個に蒸留し、有機相から有機溶媒及び油、水相から水及びNa2Sをそれぞれ回収する工程と
を含む方法を提供する。
以下に記載の脱硫実施例を、重油又は残油として特に知られている、石油留分(残渣)の代表例であるカーボンブラック給油(CBFO)において行った。CBFO脱硫実験は、ナトリウム金属を用いて行った。脱硫プロセスの詳細な記載は、同時係属中のインド特許出願第845/MUM/2011号に与えられている。このように、CBFOの脱硫をナトリウムを用いて予備的に行うが、補助成分としての水素及び有機溶媒キシレンに関しては、プロセス変形例が含まれている。このように、収率及び副生成物形成の観点で水素及びキシレンの脱硫プロセスへの影響を研究するために、以下のスキームを調査した:
実施例1:キシレンの存在下及びH2の非存在下でのナトリウムによる脱硫
実施例2:キシレンの存在下及びH2の存在下でのナトリウムによる脱硫
実施例3:キシレンの非存在下及びH2の非存在下でのナトリウムによる脱硫
実施例4:キシレンの非存在下及びH2の存在下でのナトリウムによる脱硫
約210gのCBFO及び90mlのキシレンを高圧反応器に入れた。これは、70:30(重量:体積)のCBFO:キシレン比に相当する。反応器に水素を添加しなかった。次いで化学量論量のナトリウム金属を反応器に添加した。次いで、約290℃の温度及び1時間の滞留時間で反応を行った。反応後、内容物を冷却及びデカントした。これにより、2つの別の相、液体相としての脱硫されたCBFO及び半固体相としてのNa2S+CBFOのスラッジを形成させた。デカントされたCBFOを秤量した。このCBFO及びスラッジの収率を表1に与える。
約210gのCBFO及び90mlのキシレンを高圧反応器に入れ、約300psigの水素を反応器に添加した。
約210gのCBFOを入れ、キシレンも水素も添加しなかった。
約210gのCBFOを入れ、キシレンを添加しなかったが、約300psigの水素を反応器に添加した。
この場合には、約285gのCBFO及び15mlのキシレンを高圧反応器に入れ、約300psigの水素を反応器に添加した。これに、化学量論量のナトリウム金属を添加した。1時間の滞留時間の間、反応温度を約290℃に保った。こうして、反応後、CBFOを冷却及びデカントした。このスキームによってもまた、相当量のスラッジ(Na2S+CBFO)相がもたらされた。デカントされたCBFOを秤量した。CBFO及びスラッジの収率を表番号2に提供する。
210gのCBFOを90mlのキシレンと混合した。これにより、CBFO:キシレン=70:30(重量:体積基準)としての混合物を得た。混合物を激しく混合し、次いで高圧反応器に移した。化学量論量のナトリウム金属を別途秤量した。次いでナトリウム金属を小片に切断し、反応器においてCBFO/キシレン混合物に添加した。次いで反応器を約300psiの水素で加圧した。その後、反応器を1時間にわたって290℃の温度に加熱した。反応後、溶液全体を室温まで冷却させ、次いでCBFOをデカントした。CBFO及びスラッジの量を分けて秤量した。脱硫の百分率をCBFO及びスラッジの百分率での収率と併せて以下に与える。
この実施例においては、実施例6に記載した加熱脱水の工程を回避した、すなわち、硫化ナトリウムの溶液を固体硫化ナトリウムに変換しなかった。その代わり、実施例1において得られた水層を、活性炭を用いて直接濾過し、これにより、透明な、黄色に着色した溶液の形成をもたらした。次いで、約25mlのこの溶液を三ツ口丸底フラスコに入れ、還流しながら60〜70Cの温度で加熱した。次いで圧縮空気をこの温度でこの溶液中に30分にわたってパージした。30分後、溶液を次いでビーカー中に移し、160℃で加熱して固体硫化ナトリウムを再生した。
Claims (6)
- 石油残渣の脱硫の際に形成された硫化ナトリウム(Na2S)の単離及び精製のための方法であって、以下の工程、
石油残渣の脱硫の際に得られたNa2Sを含有するスラッジを、石油残渣を溶解することが可能な少なくとも1種の有機溶媒と水との混合物で処理する工程、
処理されたスラッジを、石油を含有する有機相と、Na2Sを含有する水相とに分離させる工程、及び
前記水相を蒸留し、単離されたNa2Sを得、続いて精製する工程、
を含むことを特徴とする方法。 - 石油残渣の脱硫から由来するスラッジからNa2S及び油を回収するための方法であって、以下の工程、
少なくとも1種の有機溶媒と水との混合物を調製する工程、
約25〜100℃の温度で約20分〜2時間にわたって撹拌しながら前記混合物をスラッジに添加して、溶液を得る工程、
前記溶液を分離漏斗に移して静置させ、Na2Sを含有する水相と石油を含有する有機相との混合物を得る工程、
2相のそれぞれを別個に蒸留し、前記有機相から有機溶媒及び油、前記水相から水及びNa2Sをそれぞれ回収する工程、
を含むことを特徴とする方法。 - 前記有機溶媒が、アルカン、芳香族炭化水素、アルケン、環状アルケン、アルキン及びこれらの混合物からなる群から選択される、請求項1又は2に記載の方法。
- 前記有機溶媒が、キシレン、n−ヘキサン、シクロヘキサン、ヘプタン、ヘキサン、ヘプテン、オクタン及びトルエンからなる群から選択される少なくとも1種の炭化水素溶媒である、請求項1又は2に記載の方法。
- 有機溶媒対水の割合が、0.5:1〜2:1である、請求項1又は2に記載の方法。
- 硫化ナトリウム(Na2S)が、Na2SO3に更に酸化され;該酸化が、Na2Sを蒸留水に溶解させて溶液を得;前記溶液を約50〜80℃の温度で還流し;約20分〜120分にわたって前記溶液を通して圧縮空気をパージし;前記溶液を約140〜180℃の温度で加熱して固体亜硫酸ナトリウム(Na2SO3)粉末を得ることを含む、請求項1又は2に記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IN1235MU2011 | 2011-04-15 | ||
IN1235/MUM/2011 | 2011-04-15 | ||
PCT/IN2012/000263 WO2012147097A2 (en) | 2011-04-15 | 2012-04-12 | A process for separation and purification of sodium sulfide |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2014517798A JP2014517798A (ja) | 2014-07-24 |
JP5824137B2 true JP5824137B2 (ja) | 2015-11-25 |
Family
ID=47072834
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2014504453A Active JP5824137B2 (ja) | 2011-04-15 | 2012-04-12 | 硫化ナトリウムの分離及び精製方法 |
Country Status (12)
Country | Link |
---|---|
US (1) | US9114988B2 (ja) |
EP (1) | EP2696954B1 (ja) |
JP (1) | JP5824137B2 (ja) |
KR (1) | KR101897454B1 (ja) |
CN (2) | CN106904641B (ja) |
BR (1) | BR112013026498B1 (ja) |
CA (1) | CA2833208C (ja) |
ES (1) | ES2897456T3 (ja) |
HU (1) | HUE057015T2 (ja) |
MX (1) | MX356615B (ja) |
RU (1) | RU2561625C2 (ja) |
WO (1) | WO2012147097A2 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9873797B2 (en) | 2011-10-24 | 2018-01-23 | Aditya Birla Nuvo Limited | Process for the production of carbon black |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9475998B2 (en) | 2008-10-09 | 2016-10-25 | Ceramatec, Inc. | Process for recovering alkali metals and sulfur from alkali metal sulfides and polysulfides |
US9546325B2 (en) | 2009-11-02 | 2017-01-17 | Field Upgrading Limited | Upgrading platform using alkali metals |
US9688920B2 (en) | 2009-11-02 | 2017-06-27 | Field Upgrading Limited | Process to separate alkali metal salts from alkali metal reacted hydrocarbons |
US9441170B2 (en) | 2012-11-16 | 2016-09-13 | Field Upgrading Limited | Device and method for upgrading petroleum feedstocks and petroleum refinery streams using an alkali metal conductive membrane |
US9512368B2 (en) | 2009-11-02 | 2016-12-06 | Field Upgrading Limited | Method of preventing corrosion of oil pipelines, storage structures and piping |
KR101897454B1 (ko) | 2011-04-15 | 2018-09-12 | 아디트야 비를라 사이언스 앤 테크놀로지 컴퍼니 리미티드 | 황화나트륨을 분리 및 정제하는 방법 |
JP6272295B2 (ja) | 2012-03-30 | 2018-01-31 | アディティア ビルラ サイエンス アンド テクノロジー カンパニー プライベート リミテッド | 硫黄分を低減したカーボンブラック粉末を得る方法 |
MX358116B (es) | 2012-07-13 | 2018-08-06 | Field Upgrading Ltd | Produccion de petroleo integrada y mejora utilizando un metal alcalino fundido. |
EP2986691A4 (en) * | 2013-04-15 | 2017-03-29 | Field Upgrading Limited | Process to separate alkali metal salts from alkali metal reacted hydrocarbons |
WO2016059725A1 (ja) * | 2014-10-17 | 2016-04-21 | Jfeエンジニアリング株式会社 | 石油精製廃棄物処理装置及び石油精製廃棄物処理方法 |
US20160377052A1 (en) * | 2015-06-29 | 2016-12-29 | General Electric Company | Blade root section for a modular rotor blade and method of manufacturing same |
US10436068B2 (en) * | 2016-02-12 | 2019-10-08 | General Electric Company | Flowpath contouring |
CN116374961B (zh) * | 2023-03-14 | 2024-06-07 | 山东瑞福锂业有限公司 | 一种提纯工业级无水硫化钠的方法 |
Family Cites Families (31)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3165378A (en) | 1961-06-26 | 1965-01-12 | Joy S Greenawalt | Conversion of sodium sulfide to sodium sulfite |
US3320157A (en) * | 1964-11-16 | 1967-05-16 | Exxon Research Engineering Co | Desulfurization of residual crudes |
US3565792A (en) | 1968-06-07 | 1971-02-23 | Frank B Haskett | Cyclic process for desulfurizing crude petroleum fractions with sodium |
US3698860A (en) | 1968-10-30 | 1972-10-17 | Kaoru Shiba | Method for converting sodium sulfide to sodium sulfite |
US3657064A (en) | 1969-09-18 | 1972-04-18 | Owens Illinois Inc | Direct oxidative conversion of sodium sulfide to sodium sulfite by absorbing the heat of reaction in a fluidized bed system using adiabatic cooling |
JPS5012871B1 (ja) | 1969-11-21 | 1975-05-15 | ||
US3755149A (en) * | 1971-06-09 | 1973-08-28 | Sun Oil Co Pennsylvania | Process for desulfurizing petroleum resids |
JPS5130877B2 (ja) * | 1972-05-26 | 1976-09-03 | ||
US3859425A (en) * | 1972-11-27 | 1975-01-07 | Stauffer Chemical Co | Process for recovery of sulfur values |
JPS5112480B2 (ja) * | 1973-01-30 | 1976-04-20 | ||
JPS543310B2 (ja) * | 1973-06-06 | 1979-02-21 | ||
JPS5618710B2 (ja) * | 1973-08-20 | 1981-05-01 | ||
US4248693A (en) * | 1979-11-15 | 1981-02-03 | Rollan Swanson | Process for recovering hydrocarbons and other values from tar sands |
JPS6155283A (ja) * | 1984-08-21 | 1986-03-19 | 北陽製紙株式会社 | 亜硫酸ソ−ダ消解廃液の再生方法 |
JPH0637761B2 (ja) | 1985-12-16 | 1994-05-18 | 義之 大串 | コンクリ−ト構造体 |
CN86104945A (zh) * | 1986-07-31 | 1988-02-10 | 张新球 | 生产氢氧化物、硫代硫酸盐、硫酸盐、硫磺的方法 |
JPH0626402B2 (ja) | 1990-10-24 | 1994-04-06 | 松下電送株式会社 | ファクシミリ放送受信装置 |
US6210564B1 (en) * | 1996-06-04 | 2001-04-03 | Exxon Research And Engineering Company | Process for desulfurization of petroleum feeds utilizing sodium metal |
US7588680B1 (en) * | 2003-04-17 | 2009-09-15 | Trans Ionics Corporation | Desulphurization of petroleum streams using metallic sodium |
US7192516B2 (en) | 2003-04-17 | 2007-03-20 | Trans Ionics Corporation | Desulfurization of petroleum streams using metallic sodium |
US7632396B2 (en) * | 2004-07-14 | 2009-12-15 | Exxonmobil Research And Engineering Company | Method for reducing the level of elemental sulfur and total sulfur in hydrocarbon streams |
JP4637761B2 (ja) | 2006-02-07 | 2011-02-23 | パナソニック株式会社 | 半導体装置およびその製造方法 |
CA2657780C (en) * | 2006-07-19 | 2012-02-07 | Uop Llc | A hydrocarbon desulfurization process |
CN100406092C (zh) * | 2006-11-03 | 2008-07-30 | 中国科学院长春应用化学研究所 | 一种水溶液中离子液体富集工艺 |
EP2334428B1 (en) * | 2007-11-28 | 2018-04-04 | Chevron U.S.A., Inc. | Process for recovering base metals from used hydroprocessing catalyst |
CN101391940B (zh) | 2008-10-27 | 2011-07-20 | 西安应化生物技术有限公司 | 香紫苏醇的分离方法 |
CN101445458B (zh) | 2009-01-06 | 2010-10-06 | 烟台巨力异氰酸酯有限公司 | 一种二硝基甲苯相分离方法 |
CN101481307B (zh) | 2009-01-13 | 2010-06-02 | 湖南瑞源石化股份有限公司 | 一种从反应产物中分离出乙酸和乙酸仲丁酯的方法 |
US8404106B2 (en) * | 2009-12-18 | 2013-03-26 | Exxonmobil Research And Engineering Company | Regeneration of alkali metal reagent |
US8901537B2 (en) | 2010-12-21 | 2014-12-02 | Intel Corporation | Transistors with high concentration of boron doped germanium |
KR101897454B1 (ko) | 2011-04-15 | 2018-09-12 | 아디트야 비를라 사이언스 앤 테크놀로지 컴퍼니 리미티드 | 황화나트륨을 분리 및 정제하는 방법 |
-
2012
- 2012-04-12 KR KR1020137028911A patent/KR101897454B1/ko active IP Right Grant
- 2012-04-12 CA CA2833208A patent/CA2833208C/en active Active
- 2012-04-12 MX MX2013012042A patent/MX356615B/es active IP Right Grant
- 2012-04-12 US US14/111,048 patent/US9114988B2/en active Active
- 2012-04-12 RU RU2013150805/02A patent/RU2561625C2/ru active
- 2012-04-12 JP JP2014504453A patent/JP5824137B2/ja active Active
- 2012-04-12 ES ES12777572T patent/ES2897456T3/es active Active
- 2012-04-12 HU HUE12777572A patent/HUE057015T2/hu unknown
- 2012-04-12 EP EP12777572.4A patent/EP2696954B1/en active Active
- 2012-04-12 CN CN201710168697.7A patent/CN106904641B/zh active Active
- 2012-04-12 WO PCT/IN2012/000263 patent/WO2012147097A2/en active Application Filing
- 2012-04-12 BR BR112013026498-5A patent/BR112013026498B1/pt active IP Right Grant
- 2012-04-12 CN CN201280018300.1A patent/CN103635241B/zh active Active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9873797B2 (en) | 2011-10-24 | 2018-01-23 | Aditya Birla Nuvo Limited | Process for the production of carbon black |
Also Published As
Publication number | Publication date |
---|---|
CA2833208C (en) | 2016-06-28 |
JP2014517798A (ja) | 2014-07-24 |
US20140030185A1 (en) | 2014-01-30 |
CN106904641B (zh) | 2019-07-09 |
CN103635241B (zh) | 2017-04-19 |
CA2833208A1 (en) | 2012-11-01 |
WO2012147097A3 (en) | 2013-03-21 |
CN103635241A (zh) | 2014-03-12 |
MX2013012042A (es) | 2014-05-27 |
KR101897454B1 (ko) | 2018-09-12 |
RU2013150805A (ru) | 2015-05-20 |
CN106904641A (zh) | 2017-06-30 |
EP2696954B1 (en) | 2021-08-25 |
ES2897456T3 (es) | 2022-03-01 |
RU2561625C2 (ru) | 2015-08-27 |
US9114988B2 (en) | 2015-08-25 |
BR112013026498B1 (pt) | 2020-12-15 |
KR20140026450A (ko) | 2014-03-05 |
EP2696954A2 (en) | 2014-02-19 |
WO2012147097A2 (en) | 2012-11-01 |
EP2696954A4 (en) | 2015-01-14 |
MX356615B (es) | 2018-06-06 |
HUE057015T2 (hu) | 2022-04-28 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5824137B2 (ja) | 硫化ナトリウムの分離及び精製方法 | |
CN109563436B (zh) | 通过热处理纯化原料 | |
JP4866351B2 (ja) | 直接石炭液化のためのプロセス | |
RU2552617C2 (ru) | Способ извлечения металлов из потока, обогащенного углеводородами и углеродсодержащими остатками | |
CA2549358C (en) | Heavy oil upgrading process | |
WO2014003943A1 (en) | Decontamination of deoxygenated biomass-derived pyrolysis oil using ionic liquids | |
US10427069B2 (en) | Process for upgrading biomass derived products using liquid-liquid extraction | |
KR101794623B1 (ko) | 안수 중에 함유된 타르 에멀전 제거방법 및 장치 | |
CA2911456C (en) | Process for upgrading biomass derived products using liquid-liquid extraction | |
CN104718276A (zh) | 用于通过从含有机过氧化物的未加工的裂化汽油馏分回收高纯度苯来制备贫苯汽油的方法 | |
WO2001040406A1 (en) | A process for recovering hydrocarbons from a carbon containing material | |
JP2007302788A (ja) | 水素化分解生成物の製造方法、プラスチックの処理方法及びベンゼン類の製造方法 | |
JPH0220593A (ja) | 重質炭化水素をより軽質の炭化水素に転化する方法 | |
US2881221A (en) | Purification of cresylic acids | |
JP2019026612A (ja) | ナフタレン含有油の脱酸方法 | |
EP4334274A1 (en) | Contaminant removal from coal tar-derived crude phenols | |
EP3481524A1 (en) | Process for upgrading biomass derived products using liquid-liquid extraction | |
JP2007291289A (ja) | プラスチックの処理方法およびその処理装置ならびにベンゼン類の製造方法およびその製造装置 | |
JP2017193662A (ja) | 軽油の精製方法およびc8芳香族炭化水素の製造方法 | |
JPS61276889A (ja) | 溶剤精製炭の脱灰における溶剤回収方法 | |
SK286116B6 (sk) | Spôsob regenerácie opotrebovaných minerálnych olejov |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20150212 |
|
A601 | Written request for extension of time |
Free format text: JAPANESE INTERMEDIATE CODE: A601 Effective date: 20150511 |
|
A601 | Written request for extension of time |
Free format text: JAPANESE INTERMEDIATE CODE: A601 Effective date: 20150611 |
|
A601 | Written request for extension of time |
Free format text: JAPANESE INTERMEDIATE CODE: A601 Effective date: 20150710 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20150811 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20150909 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20151008 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 5824137 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |