CN114931927B - Adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil and preparation method thereof - Google Patents
Adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil and preparation method thereof Download PDFInfo
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- CN114931927B CN114931927B CN202210473567.5A CN202210473567A CN114931927B CN 114931927 B CN114931927 B CN 114931927B CN 202210473567 A CN202210473567 A CN 202210473567A CN 114931927 B CN114931927 B CN 114931927B
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- adsorbent
- acid
- aromatic hydrocarbon
- oxide
- gasoline
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 61
- 150000004945 aromatic hydrocarbons Chemical class 0.000 title claims abstract description 59
- 239000002283 diesel fuel Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 claims abstract description 46
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 38
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 35
- 238000000926 separation method Methods 0.000 claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 20
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical class [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003513 alkali Substances 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 19
- 229910052751 metal Chemical class 0.000 claims abstract description 18
- 239000002184 metal Chemical class 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000003921 oil Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 238000003795 desorption Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 3
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- 239000002131 composite material Substances 0.000 claims description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 13
- 230000032683 aging Effects 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical group CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 7
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 6
- 235000019260 propionic acid Nutrition 0.000 claims description 5
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 5
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 3
- 150000007530 organic bases Chemical class 0.000 claims description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 3
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 3
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 2
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 2
- 150000002484 inorganic compounds Chemical class 0.000 claims 1
- 150000002894 organic compounds Chemical class 0.000 claims 1
- 229910002027 silica gel Inorganic materials 0.000 description 15
- 239000000741 silica gel Substances 0.000 description 15
- 239000012065 filter cake Substances 0.000 description 14
- 238000011156 evaluation Methods 0.000 description 12
- 239000000499 gel Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 238000011068 loading method Methods 0.000 description 5
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 5
- WZNFFVCEJNSSPV-UHFFFAOYSA-M [OH-].[Na+].CCCCN Chemical compound [OH-].[Na+].CCCCN WZNFFVCEJNSSPV-UHFFFAOYSA-M 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- PZAGQUOSOTUKEC-UHFFFAOYSA-N acetic acid;sulfuric acid Chemical compound CC(O)=O.OS(O)(=O)=O PZAGQUOSOTUKEC-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- SSNBZPCCTUTRBD-UHFFFAOYSA-N propanoic acid;sulfuric acid Chemical compound CCC(O)=O.OS(O)(=O)=O SSNBZPCCTUTRBD-UHFFFAOYSA-N 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- LYEWAIRXZWODSJ-UHFFFAOYSA-M [OH-].[K+].CCCCN Chemical compound [OH-].[K+].CCCCN LYEWAIRXZWODSJ-UHFFFAOYSA-M 0.000 description 1
- WJGAPUXHSQQWQF-UHFFFAOYSA-N acetic acid;hydrochloride Chemical compound Cl.CC(O)=O WJGAPUXHSQQWQF-UHFFFAOYSA-N 0.000 description 1
- IZQZNLBFNMTRMF-UHFFFAOYSA-N acetic acid;phosphoric acid Chemical compound CC(O)=O.OP(O)(O)=O IZQZNLBFNMTRMF-UHFFFAOYSA-N 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000008367 deionised water Chemical class 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- FADIYVNKNQZKMK-UHFFFAOYSA-N nitric acid;propanoic acid Chemical compound O[N+]([O-])=O.CCC(O)=O FADIYVNKNQZKMK-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- XGFABUPTUPKRQI-UHFFFAOYSA-M potassium;n,n-diethylethanamine;hydroxide Chemical compound [OH-].[K+].CCN(CC)CC XGFABUPTUPKRQI-UHFFFAOYSA-M 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- ZGMWRQIARRVYDR-UHFFFAOYSA-M sodium;n,n-diethylethanamine;hydroxide Chemical compound [OH-].[Na+].CCN(CC)CC ZGMWRQIARRVYDR-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical class O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
-
- 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
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/06—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents with moving sorbents or sorbents dispersed in the oil
- C10G25/08—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents with moving sorbents or sorbents dispersed in the oil according to the "moving bed" method
-
- 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
- C10G2300/1037—Hydrocarbon fractions
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/30—Aromatics
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses an adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil and a preparation method thereof, wherein the adsorbent consists of active oxides, and comprises active silicon oxide and high-dispersion metal oxide, wherein the mass content of the metal oxide is 0.5-50%, and the preparation method of the adsorbent comprises the following steps: 1) Synthesizing oxide gel by taking sodium silicate, inorganic acid and metal salt as raw materials, and then mixing and dissolving the washed oxide gel and inorganic-organic compound alkali to obtain high-dispersion metal oxide sol; 2) Mixing the high-dispersion metal oxide sol with inorganic-organic compound acid to obtain active gel; 3) Filtering, washing, drying and roasting the active gel to obtain the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil. The adsorbent is applied to the simulated moving bed aromatic hydrocarbon adsorption separation process, the catalyst-to-oil ratio is less than 1.5, and the desorption/adsorption speed is less than 1.2.
Description
Technical Field
The invention relates to an adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil and a preparation method thereof.
Background
Through the sustainable development in recent years, although the refining industry in China becomes a national economic pulse and safe post industry, the refining industry is a problem to be solved urgently for refining enterprises, wherein the problems are that the productivity is excessive, the product homogenization is serious, the enterprise development innovation is insufficient, the environmental protection pressure is high, the foreign market competition is serious and the like. The oil is suitable for oil, the alkene is suitable for alkene and the aromatic is suitable for aromatic, which becomes the aim pursued by various large refining enterprises, but the total technical level is still not high, the innovation capability is poor, the technical content and the added value of the product are low, and the maximization and the reasonable utilization of the value of the oil are not really realized.
The Simulated Moving Bed (SMB) is used for carrying out adsorption separation on gasoline and diesel oil to obtain high-purity aromatic hydrocarbon and high-purity non-aromatic hydrocarbon components, so that molecular management of the gasoline and diesel oil components can be realized, market demand change can be more targeted and dealt with, and the subsequent conversion process of aromatic hydrocarbon and non-aromatic hydrocarbon can be coupled, so that the oriented conversion of gasoline and diesel oil to chemicals can be realized, and the economic benefit can be improved. The SMB adsorption separation process needs spherical particle adsorbent with a certain size range, and the formed adsorbent contains a large amount of binder, so that the problems of small adsorption capacity, low adsorption rate and poor adsorption effect can be generated.
Patent CN106140078B discloses a preparation method of a bimetallic aromatic adsorbent, which uses sodium silicate, inorganic acid, deionized water and metal salt as raw materials to prepare the bimetallic aromatic adsorbent which is spherical particles, wherein the metal comprises alkaline earth metal and transition metal, can effectively adsorb aromatic hydrocarbon in solvent oil, has an aromatic hydrocarbon removal rate of more than 95%, and is suitable for adsorption separation of high boiling point solvent oil aromatic hydrocarbon. Patent CN105536695B discloses an adsorbent for adsorbing and separating polycyclic aromatic hydrocarbon and a preparation method thereof, wherein the adsorbent consists of a Y molecular sieve carrier and metal ions exchanged on the Y molecular sieve carrier according to a specific sequence, and the adsorbent has a strong adsorption capacity for polycyclic aromatic hydrocarbon, can effectively adsorb and separate polycyclic aromatic hydrocarbon in diesel oil, and has a removal rate up to 80%. Patent CN105289466B discloses an adsorbent for adsorbing and separating polycyclic aromatic hydrocarbon in diesel oil and a preparation method thereof, wherein the adsorbent comprises silica gel with adjustable pore diameter or modified silica gel loaded with metal, the loaded metal is one or more of Cu, ni, al, fe, co, cr, ba, ag, the adsorbent has strong adsorption capacity to polycyclic aromatic hydrocarbon in diesel oil, the selectivity is high, and the adsorbent can be regenerated and reused.
The patent of the aromatic hydrocarbon adsorbent mainly solves the problem of the adsorption separation purity of aromatic hydrocarbon, but the use amount of the adsorption separation desorber is larger, the desorption speed of aromatic hydrocarbon is slow, the adsorption separation energy consumption is high, and the economic benefit of an industrial application device can be reduced.
Disclosure of Invention
The invention aims to solve the technical problems that the desorption speed of aromatic hydrocarbon in an adsorbent is low, the consumption of desorber in the application process of the gasoline and diesel aromatic hydrocarbon adsorbent is high, the separation energy consumption is high, and the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel is provided with an aromatic hydrocarbon adsorption active center with a high connectivity silica-metal oxide framework, and the catalyst-oil ratio (desorber/raw oil) is less than 1.5 and the desorption/adsorption speed is less than 1.2 when the adsorbent is applied to adsorbing and separating aromatic hydrocarbon in gasoline and diesel.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention provides a preparation method of an adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil, which comprises the following steps:
1) Synthesizing oxide gel by using sodium silicate, metal salt and inorganic acid as raw materials, adjusting pH value to be 5-12, filtering, washing, adding into organic-inorganic composite alkali solution, adjusting pH value to be more than 10, heating and stirring until the solution is dissolved, depolymerizing agglomerated metal, and re-coordinating metal atoms and silicon atoms to obtain high-dispersion metal oxide sol;
2) Mixing the high-dispersion metal oxide sol with organic-inorganic compound acid, regulating the pH value to be less than 2.5, improving the connectivity of a silica-metal oxide framework, and then heating and aging to obtain active oxide gel;
3) Filtering, washing, drying and roasting the active oxide gel to obtain the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil;
the adsorbent consists of active oxides, including active silicon oxide and high-dispersion metal oxide, wherein the mass content of the metal oxide is 0.5% -50%, and the metal oxide is one of germanium oxide, tin oxide, titanium oxide, zirconium oxide, manganese oxide and vanadium oxide.
In the technical scheme of the preparation method of the adsorbent, the mass fraction of silicon dioxide in the sodium silicate in the step 1) is 5-30%; the metal salt is one of germanium chloride, tin chloride, stannous sulfate, titanium chloride, titanium nitrate, titanium sulfate, zirconium chloride, zirconium nitrate and zirconium sulfate; the inorganic acid is one of hydrochloric acid, nitric acid, sulfuric acid and phosphoric acid, and the mass fraction is 5-20%; the mass fraction of the organic-inorganic composite alkali is 5-20%, the inorganic alkali is one of sodium hydroxide and potassium hydroxide, the organic alkali is one of triethylamine and n-butylamine, and the mass ratio of the inorganic alkali is as follows: organic base = 1: (0.1-5), the heating temperature is preferably 50-100 ℃.
In the aromatic hydrocarbon adsorption preparation method, in the step 2), the mass fraction of the organic-inorganic composite acid is 5-20%, the inorganic acid is one of hydrochloric acid, nitric acid, sulfuric acid and phosphoric acid, the organic acid is one of acetic acid and propionic acid, and the mass ratio of the inorganic acid is as follows: organic base = 1: (0.1-5), wherein the aging temperature is 20-80 ℃ and the aging time is 1-20h.
The invention also provides an adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil obtained by the preparation method.
Further, the invention also provides application of the adsorbent in a process for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil. The process for absorbing and separating aromatic hydrocarbon in gasoline and diesel oil is preferably a fixed bed absorption and separation process, a multi-tower parallel absorption and separation process and a simulated moving bed absorption and separation process.
In the application of the adsorbent in the adsorption separation of aromatic hydrocarbon in gasoline and diesel oil, the simulated moving bed adsorption separation process is a countercurrent simulated moving bed adsorption separation process, the adsorption bed layer is 8-24 layers, preferably 8-16 layers, the adsorption separation temperature is 40-120 ℃, preferably 50-80 ℃, the desorbant is a mixture of alkane and aromatic hydrocarbon, preferably methylcyclohexane and toluene, and the mass fraction of toluene is 10% -50%.
The adsorbent is preferably used in the process for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil by the simulated moving bed, the purity of the aromatic hydrocarbon component of the product is more than 98%, the purity of the non-aromatic hydrocarbon component is more than 98%, the ratio of the catalyst to the oil is less than 1.5, and the desorption/adsorption speed is less than 1.2.
The invention has the beneficial effects that: by the application of the adsorbent in adsorption separation of aromatic hydrocarbon in gasoline and diesel oil, the separation energy consumption is reduced by 20% compared with the conventional metal modified silicon oxide adsorbent according to the reduction range of the catalyst-to-oil ratio.
Detailed Description
The following describes the technical scheme of the invention in conjunction with examples, but is not limited to these examples.
The evaluation performance data of the adsorbents in examples were measured by: the gasoline and diesel oil are used as raw materials, and the aromatic hydrocarbon content of the fraction section is 15-70%. Loading the adsorbent into a simulated moving bed, and carrying out adsorption separation on aromatic hydrocarbon into a countercurrent simulated moving bed adsorption separation process, wherein the adsorption bed layer is 8-24 layers, preferably 8-16 layers, the adsorption separation temperature is 40-120 ℃, preferably 50-80 ℃, the desorbant is a mixture of alkane and aromatic hydrocarbon, preferably methylcyclohexane and toluene, and the mass fraction of toluene is 10% -50%. Two materials are extracted from the simulated moving bed, one material is rich in aromatic hydrocarbon components, the other material is rich in non-aromatic hydrocarbon components, and the purity and the desorption ratio of the two materials are analyzed.
Example 1
(1) Forming a highly dispersed metal oxide sol: preparing 10kg of sodium silicate solution with the mass fraction of 12% and a proper amount of dilute sulfuric acid solution with the mass fraction of 15%, dissolving 14.8g of germanium chloride into the dilute sulfuric acid solution, slowly adding the dilute sulfuric acid solution into the sodium silicate solution, vigorously stirring in the adding process, adjusting the pH value to 7, filtering and washing to obtain a filter cake, and mixing the filter cake with sodium hydroxide-triethylamine composite alkali solution with the mass fraction of 5%, wherein the mass ratio of sodium hydroxide: triethylamine=1:2, regulating the pH value to be more than 10, heating to 50 ℃, stirring and dissolving to obtain the high-dispersion metal oxide sol.
(2) Forming an active silica gel; preparing a proper amount of sulfuric acid-acetic acid composite acid solution with the mass fraction of 5%, wherein the mass ratio of sulfuric acid: acetic acid=1:5, and mixing with the high dispersion metal oxide sol obtained in the step (1), regulating the pH value to be less than 2.5, heating to 50 ℃, stirring and aging for 12 hours, thus obtaining the active silica gel.
(3) Filtering, washing, drying at 150 ℃ for 12h and roasting at 550 ℃ for 4h the active oxide gel obtained in the step (2) to obtain the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil.
(4) Evaluation of adsorbent: the hydrogenation catalytic diesel is used as a raw material, the mass fraction of aromatic hydrocarbon components is 30.5%, an adsorbent is filled into a simulated moving bed, the aromatic hydrocarbon adsorption separation is a countercurrent simulated moving bed adsorption separation process, the adsorption bed layer is 12 layers, the adsorption separation temperature is 60 ℃, and the mass fraction of desorbent methylcyclohexane and toluene is 20%. Two materials are extracted from the simulated moving bed, one material is rich in aromatic hydrocarbon components, the other material is rich in non-aromatic hydrocarbon components, and the purity and the catalyst-oil ratio of the two materials are analyzed. The evaluation results are shown in Table 1.
Example 2
(1) Forming a highly dispersed metal oxide sol: preparing 10kg of sodium silicate solution with the mass fraction of 12% and a proper amount of diluted hydrochloric acid solution with the mass fraction of 15%, dissolving 207.4g of stannic chloride into the diluted hydrochloric acid solution, slowly adding the diluted hydrochloric acid solution into the sodium silicate solution, vigorously stirring in the adding process, adjusting the pH value to 8, filtering and washing to obtain a filter cake, and mixing the filter cake with sodium hydroxide-n-butylamine composite alkali solution with the mass fraction of 10%, wherein the mass ratio of sodium hydroxide: n-butylamine=1:0.1, adjusting the pH value to be more than 10, heating to 80 ℃, stirring and dissolving to obtain the high-dispersion metal oxide sol.
(2) Forming an active silica gel; preparing a proper amount of hydrochloric acid-acetic acid composite acid solution with the mass fraction of 10%, wherein the mass ratio of hydrochloric acid: acetic acid=1:0.1, and mixing with the high dispersion metal oxide sol obtained in the step (1), regulating the pH value to be less than 2.5, heating to 80 ℃, stirring and aging for 1h to obtain the active silica gel.
(3) Filtering, washing, drying at 120 ℃ for 12h and roasting at 500 ℃ for 6h the active oxide gel obtained in the step (2) to obtain the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil.
(4) Evaluation of adsorbent: the same as in example 1.
Example 3
(1) Forming a highly dispersed metal oxide sol: preparing 10kg of sodium silicate solution with the mass fraction of 12% and a proper amount of dilute nitric acid solution with the mass fraction of 15%, dissolving 170.9g of stannous sulfate into the dilute nitric acid solution, slowly adding the dilute nitric acid solution into the sodium silicate solution, vigorously stirring in the adding process, adjusting the pH value to 10, filtering and washing to obtain a filter cake, and mixing the filter cake with a potassium hydroxide-triethylamine composite alkali solution with the mass fraction of 15%, wherein the mass ratio is potassium hydroxide: triethylamine=1:5, regulating the pH value to be more than 10, heating to 80 ℃, stirring and dissolving to obtain the high-dispersion metal oxide sol.
(2) Forming an active silica gel; preparing a proper amount of nitric acid-propionic acid composite acid solution with the mass fraction of 10%, wherein the mass ratio of nitric acid: propionic acid=1:1, mixing with the high dispersion metal oxide sol obtained in the step (1), adjusting the pH value to be less than 2.5, adjusting the temperature to 20 ℃, stirring and aging for 24 hours, and obtaining the active silica gel.
(3) Filtering, washing, drying at 150 ℃ for 12h and roasting at 550 ℃ for 4h the active oxide gel obtained in the step (2) to obtain the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil.
(4) Evaluation of adsorbent: the same as in example 1.
Example 4
(1) Forming a highly dispersed metal oxide sol: preparing 10kg of sodium silicate solution with the mass fraction of 12% and a proper amount of diluted phosphoric acid solution with the mass fraction of 15%, dissolving 853.6g of titanium chloride into the diluted phosphoric acid solution, slowly adding the diluted phosphoric acid solution into the sodium silicate solution, vigorously stirring in the adding process, adjusting the pH value to 6, filtering and washing to obtain a filter cake, and mixing the filter cake with potassium hydroxide-n-butylamine composite alkali solution with the mass fraction of 20%, wherein the mass ratio is potassium hydroxide: n-butylamine=1:1, the pH value is regulated to be more than 10, the temperature is raised to 100 ℃, and the high-dispersion metal oxide sol is obtained after stirring and dissolution.
(2) Forming an active silica gel; preparing a proper amount of phosphoric acid-acetic acid composite acid solution with the mass fraction of 20%, wherein the mass ratio of phosphoric acid: acetic acid=1:1, mixing with the high dispersion metal oxide sol obtained in the step (1), regulating the pH value to be less than 2.5, regulating the temperature to 80 ℃, stirring and aging for 6 hours, and obtaining the active silica gel.
(3) Filtering, washing, drying at 150 ℃ for 12h and roasting at 550 ℃ for 4h the active oxide gel obtained in the step (2) to obtain the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil.
(4) Evaluation of adsorbent: the same as in example 1.
Example 5
(1) Forming a highly dispersed metal oxide sol: preparing 10kg of sodium silicate solution with the mass fraction of 12% and a proper amount of dilute sulfuric acid solution with the mass fraction of 15%, dissolving 1.8kg of titanium sulfate into the dilute sulfuric acid solution, slowly adding the dilute sulfuric acid solution into the sodium silicate solution, vigorously stirring in the adding process, adjusting the pH value to 7, filtering and washing to obtain a filter cake, and mixing the filter cake with a sodium hydroxide-n-butylamine composite alkali solution with the mass fraction of 20%, wherein the mass ratio of sodium hydroxide: n-butylamine=1:0.5, adjusting the pH value to be more than 10, heating to 100 ℃, stirring and dissolving to obtain the high-dispersion metal oxide sol.
(2) Forming an active silica gel; preparing a proper amount of sulfuric acid-propionic acid composite acid solution with the mass fraction of 20%, wherein the mass ratio of sulfuric acid: propionic acid=1:5, mixing with the high dispersion metal oxide sol obtained in the step (1), adjusting the pH value to be less than 2.5, adjusting the temperature to 80 ℃, stirring and aging for 12 hours, and obtaining the active silica gel.
(3) Filtering, washing, drying at 120 ℃ for 12h and roasting at 500 ℃ for 8h the active oxide gel obtained in the step (2) to obtain the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil.
(4) Evaluation of adsorbent: the same as in example 1.
Example 6
(1) Forming a highly dispersed metal oxide sol: preparing 10kg of sodium silicate solution with the mass fraction of 12% and a proper amount of dilute sulfuric acid solution with the mass fraction of 15%, dissolving 276.9g of zirconium sulfate into the dilute sulfuric acid solution, slowly adding the dilute sulfuric acid solution into the sodium silicate solution, vigorously stirring in the adding process, adjusting the pH value to 10, filtering and washing to obtain a filter cake, and mixing the filter cake with sodium hydroxide-n-butylamine composite alkali solution with the mass fraction of 10%, wherein the mass ratio of sodium hydroxide: n-butylamine=1:0.5, adjusting the pH value to be more than 10, heating to 80 ℃, stirring and dissolving to obtain the high-dispersion metal oxide sol.
(2) Forming an active silica gel; preparing a proper amount of sulfuric acid-propionic acid composite acid solution with the mass fraction of 10%, wherein the mass ratio of sulfuric acid: propionic acid=1:0.1, mixing with the high dispersion metal oxide sol obtained in the step (1), adjusting the pH value to be less than 2.5, adjusting the temperature to 60 ℃, stirring and aging for 12 hours, and obtaining the active silica gel.
(3) Filtering, washing, drying at 120 ℃ for 12h and roasting at 500 ℃ for 4h the active oxide gel obtained in the step (2) to obtain the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil.
(4) Evaluation of adsorbent: the same as in example 1.
Example 7
(1) Forming a highly dispersed metal oxide sol: preparing 10kg of sodium silicate solution with the mass fraction of 12% and a proper amount of dilute sulfuric acid solution with the mass fraction of 15%, dissolving 418.2g of zirconium nitrate into the dilute sulfuric acid solution, slowly adding the dilute sulfuric acid solution into the sodium silicate solution, vigorously stirring in the adding process, adjusting the pH value to 10, filtering and washing to obtain a filter cake, and mixing the filter cake with sodium hydroxide-n-butylamine composite alkali solution with the mass fraction of 10%, wherein the mass ratio of sodium hydroxide: n-butylamine=1:0.5, adjusting the pH value to be more than 10, heating to 80 ℃, stirring and dissolving to obtain the high-dispersion metal oxide sol.
(2) Forming an active silica gel; preparing a proper amount of sulfuric acid-acetic acid composite acid solution with the mass fraction of 10%, wherein the mass ratio of sulfuric acid: acetic acid = 1:2, mixing the mixture with the high-dispersion metal oxide sol obtained in the step (1), adjusting the pH value to be less than 2.5, adjusting the temperature to 60 ℃, stirring and aging for 12 hours, and obtaining the active silica gel.
(3) Filtering, washing, drying at 120 ℃ for 24 hours and roasting at 600 ℃ for 4 hours the active oxide gel obtained in the step (2) to obtain the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil.
(4) Evaluation of adsorbent: the same as in example 1.
Comparative example 1
The silica adsorbent prepared by the metal salt impregnation loading method has the same metal loading as in example 1, and the adsorbent evaluation is the same as in example 1.
Comparative example 2
The silica adsorbent prepared by the metal salt impregnation loading method has the same metal loading as in example 2 and the adsorbent evaluation as in example 1.
TABLE 1 evaluation results of adsorbents
Claims (9)
1. The preparation method of the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil is characterized by comprising the following steps of:
1) Synthesizing oxide gel by using sodium silicate, metal salt and inorganic acid as raw materials, adjusting pH to be 5-12, filtering and washing, adding into inorganic-organic composite alkali solution, adjusting pH to be more than 10, heating and stirring until the inorganic-organic composite alkali solution is dissolved, depolymerizing agglomerated metal, and re-coordinating metal atoms and silicon atoms to obtain high-dispersion metal oxide sol;
2) Mixing the high-dispersion metal oxide sol with inorganic and organic compound acid, regulating the pH value to be less than 2.5, improving the connectivity of a silica-metal oxide framework, and then heating and aging to obtain active oxide gel;
3) Filtering, washing, drying and roasting the active oxide gel to obtain an adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil;
the adsorbent for adsorbing and separating aromatic hydrocarbon in gasoline and diesel oil consists of active oxide, wherein the active oxide comprises active silicon oxide and high-dispersion metal oxide, the mass content of the metal oxide is 0.5% -50%, and the metal oxide is one of germanium oxide, tin oxide, titanium oxide, zirconium oxide, manganese oxide and vanadium oxide;
the mass fraction of the inorganic-organic composite alkali in the step 1) is 5-20%, the inorganic alkali is one of sodium hydroxide and potassium hydroxide, the organic alkali is one of triethylamine and n-butylamine, and the mass ratio of the inorganic alkali is as follows: organic base = 1: (0.1-5); the mass fraction of the inorganic-organic composite acid in the step 2) is 5-20%, the inorganic acid is one of hydrochloric acid, nitric acid, sulfuric acid and phosphoric acid, the organic acid is one of acetic acid and propionic acid, and the mass ratio of the inorganic acid is as follows: organic acid = 1: (0.1-5), wherein the aging temperature is 20-80 ℃ and the aging time is 1-20h.
2. The preparation method according to claim 1, wherein the mass fraction of silica in the sodium silicate in step 1) is 5-30%; the metal salt is one of germanium chloride, tin chloride, stannous sulfate, titanium chloride, titanium nitrate, titanium sulfate, zirconium chloride, zirconium nitrate and zirconium sulfate; the inorganic acid is one of hydrochloric acid, nitric acid, sulfuric acid and phosphoric acid, and the mass fraction is 5-20%.
3. The method of claim 1, wherein the heating temperature in step 1) is 50-100 ℃.
4. An adsorbent for adsorbing and separating aromatic hydrocarbons in gasoline and diesel oil obtained by the preparation method of claim 1.
5. Use of the adsorbent of claim 4 in a process for adsorption separation of aromatic hydrocarbons in gasoline and diesel.
6. The use of claim 5, wherein the process for adsorption separation of aromatic hydrocarbons in gasoline and diesel is at least one of a fixed bed adsorption separation process, a multi-tower parallel adsorption separation process, and a simulated moving bed adsorption separation process.
7. The use according to claim 6, wherein the simulated moving bed adsorption separation process is a countercurrent simulated moving bed adsorption separation process, the adsorption bed is 8-24 layers, the adsorption separation temperature is 40-120 ℃, and the desorbent is a mixture of alkane and aromatic hydrocarbon.
8. The use according to claim 7, wherein the simulated moving bed adsorption separation process is a countercurrent simulated moving bed adsorption separation process, the adsorption bed layer is 8-16 layers, the adsorption separation temperature is 50-80 ℃, the desorbent is methylcyclohexane and toluene, and the mass fraction of toluene is 10% -50%.
9. The use according to claim 8, wherein for the simulated moving bed adsorption separation process of aromatic hydrocarbons in gasoline and diesel oil, the purity of the aromatic hydrocarbon component of the product is more than 98%, the purity of the non-aromatic hydrocarbon component is more than 98%, the catalyst-to-oil ratio is less than 1.5, and the desorption/adsorption speed is less than 1.2.
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