CN114100564A - 一种从费托合成油中脱除含氧化合物的吸附剂及制备方法 - Google Patents
一种从费托合成油中脱除含氧化合物的吸附剂及制备方法 Download PDFInfo
- Publication number
- CN114100564A CN114100564A CN202111309092.8A CN202111309092A CN114100564A CN 114100564 A CN114100564 A CN 114100564A CN 202111309092 A CN202111309092 A CN 202111309092A CN 114100564 A CN114100564 A CN 114100564A
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- Prior art keywords
- acid
- adsorbent
- fischer
- silicon dioxide
- containing compounds
- 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.)
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 55
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 54
- 239000001301 oxygen Substances 0.000 title claims abstract description 54
- 239000003463 adsorbent Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 98
- 239000003921 oil Substances 0.000 claims abstract description 49
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 37
- 239000000741 silica gel Substances 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 28
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 20
- 238000005096 rolling process Methods 0.000 claims abstract description 15
- 150000003839 salts Chemical class 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 12
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004327 boric acid Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052796 boron Inorganic materials 0.000 claims abstract description 6
- 239000000499 gel Substances 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 5
- 238000001179 sorption measurement Methods 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000012065 filter cake Substances 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 4
- 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 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 150000001299 aldehydes Chemical class 0.000 claims description 4
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 4
- 238000006392 deoxygenation reaction Methods 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 150000007513 acids Chemical class 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- 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 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000011156 evaluation Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 14
- 238000000926 separation method Methods 0.000 description 10
- 150000001336 alkenes Chemical class 0.000 description 9
- 238000012986 modification Methods 0.000 description 8
- 230000004048 modification Effects 0.000 description 8
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000000605 extraction Methods 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 4
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004711 α-olefin Substances 0.000 description 3
- 239000011651 chromium Substances 0.000 description 2
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 150000002927 oxygen compounds Chemical class 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000010944 silver (metal) Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- ATPYWZKDGYKXIM-UHFFFAOYSA-N acetic acid phosphoric acid Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.OP(O)(O)=O ATPYWZKDGYKXIM-UHFFFAOYSA-N 0.000 description 1
- PZAGQUOSOTUKEC-UHFFFAOYSA-N acetic acid;sulfuric acid Chemical compound CC(O)=O.OS(O)(=O)=O PZAGQUOSOTUKEC-UHFFFAOYSA-N 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 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
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- YYFIGOPUHPDIBO-UHFFFAOYSA-N propanoic acid;hydrochloride Chemical compound Cl.CCC(O)=O YYFIGOPUHPDIBO-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- B01J20/0218—Compounds of Cr, Mo, W
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
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- B01J20/0229—Compounds of Fe
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- B01J20/0233—Compounds of Cu, Ag, Au
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
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- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- 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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- 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
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Abstract
本发明公开了一种从费托合成油中脱除含氧化合物的吸附剂及其制备方法，该吸附剂包括质量分数为80‑95％的骨架空缺改性二氧化硅和5‑20％的粘结剂，该吸附剂的制备方法包括：1)以硅酸钠、无机酸和铝盐或硼酸为原料合成二氧化硅凝胶；2)脱除骨架铝或硼，得到骨架空缺二氧化硅凝胶；3)使用金属盐改性二氧化硅凝胶后过滤、烘干、焙烧、破碎得到二氧化硅粉体；4)将二氧化硅粉体、硅溶胶粘结剂混合后滚球成型、干燥、焙烧后制得。本发明吸附剂应用于模拟移动床脱氧工艺，可使费托合成油中含氧化合物质量分数降低至1ppm以下，且可以器内再生，重复使用。
Description
技术领域
本发明涉及吸附分离技术领域，具体涉及一种从费托合成油中脱除含氧化合物的吸附剂及其制备方法。
背景技术
费托(F-T)合成油是煤基清洁高效利用目前最有效的途径之一，F-T过程主要包括煤制合成气、合成气费托合成以及合成油品的精制加工三个主要的步骤。
费托合成油的组成复杂，主要包括α-烯烃、正构烷烃以及醇、酮、醛、酯和酸等含氧化合物，对低温合成费托油中，通常α-烯烃质量分数为40-60％，含氧化合物的质量分数为3-10％。采用模拟移动床技术将费托合成油中的烷烃和烯烃分开，不仅可以获得具有高附加值的长链烯烃，还可以生产清洁优质的航空煤油、润滑油基础油或特种溶剂油等高附加值产品。如果要将烷烃和烯烃进行分离，首先要将其中的含氧化合物进行脱除，一方面由于含氧化合物极性强于烷烃和烯烃，会优先在吸附剂上吸附，影响烯烃的吸附分离性能；另一方面含氧化合物主要以醇类为主，且含量较高，如果分离出来可直接作为高碳醇产品销售，为后续模拟移动床工艺烷烃和烯烃分离提供优质费托合成油原料。
CN111718748A公开了一种从费托合成油中脱除含氧化合物的方法，将费托合成油进行常减压分馏，得到第一段馏分、第二段馏分和第三段馏分，分别进行萃取脱氧，萃取剂为甲醇和乙醇的水溶液，可将含氧化物含量降低至100ppm以下。CN109096033A公开了一种脱除费托油合成油窄馏分中含氧化合物的方法与装置，采用隔壁萃取精馏塔或隔壁共沸精馏塔，代替传统萃取或共沸精馏的双塔结构，可将C5-C12馏分段产品的质量含量提高至99％以上。CN107338069A公开了一种脱除轻油中微量有机含氧化合物的方法，其采用固定床吸附分离的方法吸附脱除加氢处理后的费托油中含氧化合物，因为原料经过加氢，含氧化合物含量仅0.01-0.05％，脱除氧化物后含量可降至5ppm以下。CN102794181B公开了一种费托合成油加氢脱氧催化剂、其制备方法与应用，原料有机含氧化合物占 20％左右，加氢后有机含氧化合物传化率＞96％。
上述专利采用萃取精馏、固定床吸附或加氢反应的方式脱除费托合成油中含氧化合物，均没有涉及模拟移动床工艺深度脱除费托合成油中含氧化合物吸附剂。
发明内容
本发明涉及一种从费托合成油中脱除含氧化合物的吸附剂及制备方法，目的在于通过模拟移动床深度脱除费托合成油中含氧化合物至1ppm以下，为后续烷烃/烯烃分离工艺提供原料，该吸附剂对含氧化合物选择性高、吸附容量高、脱除程度深。
为解决上述技术问题，本发明通过以下技术方案来实现：
一种从费托合成油中脱除含氧化合物的吸附剂，所述吸附剂适用于模拟移动床深度脱氧工艺，使费托合成油中含氧化合物质量分数降低至1ppm以下，所述吸附剂包括质量分数为80-95％的骨架空缺改性二氧化硅和5-20％的粘结剂，孔容为0.3-1.3cm3/g，平均孔径为2-15nm；
所述的改性骨架空缺二氧化硅中的改性金属为Fe、Co、Ni、Zn、Cu、Cr、 Ag中至少一种。
上述吸附剂技术方案中，所述的改性骨架空缺二氧化硅优选由如下步骤制得：
1)以硅酸钠、无机酸，和铝盐或硼酸为原料合成二氧化硅凝胶，调节pH 值小于2.5；
2)将所述的二氧化硅凝胶先用有机-无机复合酸洗涤，脱除骨架铝或硼，再用去离子水洗涤至pH大于5，得到骨架空缺二氧化硅凝胶；
3)配制改性金属盐水溶液，与骨架空缺二氧化硅凝胶充分混合均匀后过滤，收集滤饼；
4)将上述滤饼进行烘干、焙烧、破碎得到改性骨架空缺二氧化硅粉体。
本发明还进一步提供了一种上述吸附剂的制备方法，包括以下步骤：
1)以硅酸钠、无机酸和铝盐或硼酸为原料合成二氧化硅凝胶，调节pH值小于2.5；
2)将所述的二氧化硅凝胶先用有机-无机复合酸洗涤，脱除骨架铝或硼，再用去离子水洗涤至pH大于5，得到骨架空缺二氧化硅凝胶；
3)配制改性金属盐水溶液，与骨架空缺二氧化硅凝胶充分混合均匀后过滤，收集滤饼；
4)将上述滤饼进行烘干、焙烧、破碎得到改性骨架空缺二氧化硅粉体；
5)将改性骨架空缺二氧化硅粉体、硅溶胶粘结剂混合后滚球成型、干燥、焙烧后制得。
本发明所述的从费托合成油中脱除含氧化合物的吸附剂制备方法中，步骤 1)所述硅酸钠中二氧化硅质量浓度为5-25wt％，所述无机酸为硫酸、盐酸、硝酸、磷酸中至少一种，无机酸质量浓度为5-30wt％，所述铝盐为硫酸铝、硝酸铝、异丙醇铝、偏铝酸钠中至少一种，铝盐或硼酸的添加量摩尔比为Al2O3或 B2O3:SiO2＝(0.5-2):10。
本发明所述的从费托合成油中脱除含氧化合物的吸附剂制备方法中，步骤 2)所述有机-无机复合酸为0.5-5wt％，有机酸为乙酸、丙酸中一种，无机酸为盐酸、硝酸、硫酸、磷酸中一种，质量比有机酸：无机酸＝(0.1-5)：1。
本发明所述的从费托合成油中脱除含氧化合物的吸附剂制备方法中，步骤 3)所述金属盐水溶液浓度优选为0.05-0.5mol/L，金属盐水溶液与骨架空缺二氧化硅凝胶质量比为1:1。
本发明所述的从费托合成油中脱除含氧化合物的吸附剂制备方法中，步骤 4)所述二氧化硅粉体粒径目数优选为120-500目。
本发明所述从费托合成油中脱除含氧化合物的吸附剂制备方法中，步骤5) 所述滚球成型吸附剂等效球直径尺寸优选为0.3-1.5mm。
本发明还进一步提供了上述吸附剂在脱除费托合成油含氧化合物的应用，其特中所述的含氧化合物包括醇类、酸类、酯类、醛类、酮类等有机物，脱除前质量百分含量为0.1-10％，脱除后，费托合成油中含氧化合物质量分数降低至1ppm 以下。优选应用条件为：模拟移动床费托合成油脱氧工艺，模拟移动床吸附温度为50-150℃，吸附压力为0.1-2.0MPa，吸附塔床层数8-16层，解吸剂为烷烃和醇的混合物，吸附剂器内再生重复使用。
本发明的有益效果：通过本发明吸附剂可以使通过模拟移动床深度脱除费托合成油中含氧化合物至1ppm以下，为后续烷烃/烯烃分离工艺提供原料，该吸附剂对含氧化合物选择性高、吸附容量高、脱除程度深。
具体实施方式
下面通过结合具体实施例对本发明技术方案作进一步说明。
本发明一种从费托合成油中脱除含氧化合物的吸附剂包括质量分数为 80-95％的改性骨架空缺二氧化硅和5-20％的粘结剂。在吸附剂制备过程中，以硅酸钠、无机酸和铝盐或硼酸为原料合成二氧化硅凝胶，调节pH值小于2.5；将二氧化硅凝胶先用有机-无机复合酸洗涤，脱除骨架铝或硼，再用去离子水洗涤至pH大于5，得到骨架空缺二氧化硅凝胶；配制改性金属盐水溶液，与骨架空缺二氧化硅凝胶充分混合均匀后过滤，收集滤饼；将滤饼进行烘干、焙烧、破碎得到二氧化硅粉体；二氧化硅粉体、硅溶胶粘结剂混合后滚球成型，然后干燥、焙烧得到所述从费托合成油中脱除含氧化合物的吸附剂。
在二氧化硅凝胶制备步骤中，硅酸钠中二氧化硅质量浓度为5-25wt％，无机酸为硫酸、盐酸、硝酸、磷酸中至少一种，无机酸质量浓度为5-30wt％，铝盐为硫酸铝、硝酸铝、异丙醇铝、偏铝酸钠中至少一种，铝盐或硼酸至少添加一种，添加量摩尔比为Al2O3或B2O3:SiO2＝(0.5-2):10。
在骨架空缺二氧化硅凝胶制备步骤中，有机-无机复合酸为0.5-5wt％，有机酸为乙酸、丙酸中一种，无机酸为盐酸、硝酸、硫酸、磷酸中一种，质量比有机酸：无机酸＝(0.1-5)：1。
在金属改性步骤中，金属盐为Fe、Co、Ni、Zn、Cu、Cr、Ag中至少一种，其中金属盐水溶液浓度为0.05-0.5mol/L。
在滚球成型步骤中，二氧化硅粉体粒径目数为120-500目，滚球成型吸附剂等效球直径尺寸为0.3-1.5mm。
最终制得从费托合成油中脱除含氧化合物的吸附剂，孔容为0.3-1.3cm3/g，平均孔径为2-15nm，金属含量为0.5-5wt％，应用于模拟移动床工艺，可以使费托合成油中含氧化合物质量分数降低至1ppm以下。
实施例中吸附剂的评价性能数据的测定方法为：以费托合成油中C6-C18馏分段(63-315℃)的轻油为原料，该馏分段的组成为正构烷烃、α-烯烃、含氧化合物及少量的异构烃，含氧化合物包括醇类、酸类、酯类、醛类、酮类等有机物，质量百分含量为0.1-10％,。将吸附剂装入模拟移动床中，脱氧吸附为逆流模拟移动床吸附分离工艺，吸附床层为8-24层，优选8-16层，吸附分离温度为50-150℃，优选60-100℃，解吸剂为烷烃和醇的混合物，优选甲基环己烷和乙醇，其中乙醇质量分数为10％-50％。从模拟移动床采出两股物料，一股物料为富含氧化合物组分，另一股物料为富烃类组分，其中富烃类组分中含氧化合物质量分数小于 1ppm(不计解吸剂)。
下面通过实施例说明该发明过程，但并非仅限于这些例子。
实施例1
(1)形成二氧化硅凝胶：配制10kg质量分数为16.3％的硅酸钠溶液和适量质量分数为17％的稀硫酸溶液，将930g硫酸铝溶解至稀硫酸溶液中，然后将稀硫酸溶液缓慢加入硅酸钠溶液中，加入过程中剧烈搅拌，调节pH值至小于2.5，然后在70℃下反应4小时，得到二氧化硅凝胶。
(2)形成骨架空缺二氧化硅凝胶：二氧化硅凝胶用质量分数为1％的乙酸- 硫酸复合酸充分洗涤至过滤液中不含铝，改用去离子水洗涤至过滤液pH大于5，收集滤饼。
(3)金属改性：配制0.5mol/L的硝酸铁去离子水溶液，收集的滤饼与硝酸铁溶液充分混合均匀，在50℃保持4小时，然后过滤，收集滤饼，将滤饼在120℃烘干12小时，550℃焙烧4h，然后破碎，筛分120目-200目粉体备用。
(4)滚球成型：将上述粉体与硅溶胶混合均匀，硅溶胶中氧化硅占粉体重量的10％，然后加入适量去离子水滚球成型，筛分出0.3-1.5mm颗粒，120℃烘干12h，550℃焙烧4h制得从费托合成油中脱除含氧化合物的吸附剂。
(5)吸附剂评价：以费托合成油中C6-C18馏分段(63-315℃)的轻油为原料，含氧化合物质量分数为8.6％,。将吸附剂装入模拟移动床中，脱氧吸附为逆流模拟移动床吸附分离工艺，吸附床层为12层，吸附分离温度为80℃，解吸剂甲基环己烷和乙醇，其中乙醇质量分数为20％。从模拟移动床采出两股物料，一股物料为富含氧化合物组分，另一股物料为富烃类组分，分析两股物料中含氧化合物含量。评价结果见表1所示。
实施例2
(1)形成二氧化硅凝胶：将硫酸铝改为337g硼酸，其它条件与实施例1 相同。
(2)形成骨架空缺二氧化硅凝胶：有机-无机复合酸为丙酸-硝酸，其它条件与实施例1相同。
(3)金属改性：采用0.3mol.L硝酸钴溶液，其它条件与实施例1相同。
(4)滚球成型：与实施例1相同。
(5)吸附剂评价：与实施例1相同，评价结果见表1所示。
实施例3
(1)形成二氧化硅凝胶：与实施例1相同。
(2)形成骨架空缺二氧化硅凝胶：有机-无机复合酸为丙酸-盐酸，其它条件与实施例1相同。
(3)金属改性：采用0.1mol.L硝酸镍溶液，其它条件与实施例1相同。
(4)滚球成型：与实施例1相同。
(5)吸附剂评价：与实施例1相同，评价结果见表1所示。
实施例4
(1)形成二氧化硅凝胶：将硫酸铝质量改为560g，其它条件与实施例1 相同。
(2)形成骨架空缺二氧化硅凝胶：有机-无机复合酸为乙酸-磷酸，其它条件与实施例1相同。
(3)金属改性：采用0.2mol.L硝酸锌溶液，其它条件与实施例1相同。
(4)滚球成型：与实施例1相同。
(5)吸附剂评价：与实施例1相同，评价结果见表1所示。
实施例5
(1)形成二氧化硅凝胶：将硫酸铝改为650g硼酸，其它条件与实施例1 相同。
(2)形成骨架空缺二氧化硅凝胶：与实施例1相同。
(3)金属改性：采用0.08mol.L硝酸铜溶液，其它条件与实施例1相同。
(4)滚球成型：与实施例1相同。
(5)吸附剂评价：与实施例1相同，评价结果见表1所示。
实施例6
(1)形成二氧化硅凝胶：与实施例1相同。
(2)形成骨架空缺二氧化硅凝胶：与实施例1相同。
(3)金属改性：采用0.06mol.L硝酸铬溶液，其它条件与实施例1相同。
(4)滚球成型：硅溶胶中氧化硅占粉体重量20％，其它条件与实施例1相同。
(5)吸附剂评价：与实施例1相同，评价结果见表1所示。
实施例7
(1)形成二氧化硅凝胶：与实施例1相同。
(2)形成骨架空缺二氧化硅凝胶：与实施例1相同。
(3)金属改性：采用0.05mol.L硝酸银溶液，其它条件与实施例1相同。
(4)滚球成型：硅溶胶中氧化硅占粉体重量6％，其它条件与实施例1相同。
(5)吸附剂评价：与实施例1相同，评价结果见表1所示。
表1吸附剂评价结果
Claims (10)
1.一种从费托合成油中脱除含氧化合物的吸附剂，其特征在于：所述吸附剂的孔容为0.3-1.3cm3/g，平均孔径为2-15nm，组分包括质量分数为80-95％的改性骨架空缺二氧化硅和5-20％的粘结剂；
所述的改性骨架空缺二氧化硅中的改性金属为Fe、Co、Ni、Zn、Cu、Cr、Ag中至少一种。
2.根据权利要求1所述的吸附剂，其特征在于，所述的改性骨架空缺二氧化硅由如下步骤制得：
1)以硅酸钠、无机酸，铝盐或硼酸为原料合成二氧化硅凝胶，调节pH值小于2.5；
2)将所述的二氧化硅凝胶先用有机-无机复合酸洗涤，脱除骨架铝或硼，再用去离子水洗涤至pH大于5，得到骨架空缺二氧化硅凝胶；
3)配制改性金属盐水溶液，与骨架空缺二氧化硅凝胶充分混合均匀后过滤，收集滤饼；
4)将上述滤饼进行烘干、焙烧、破碎得到改性骨架空缺二氧化硅粉体。
3.一种权利要求1所述的从费托合成油中脱除含氧化合物的吸附剂的制备方法，其特在于，包括如下步骤：
1)以硅酸钠、无机酸和铝盐或硼酸为原料合成二氧化硅凝胶，调节pH值小于2.5；
2)将所述的二氧化硅凝胶先用有机-无机复合酸洗涤，脱除骨架铝或硼，再用去离子水洗涤至pH大于5，得到骨架空缺二氧化硅凝胶；
3)配制改性金属盐水溶液，与骨架空缺二氧化硅凝胶充分混合均匀后过滤，收集滤饼；
4)将上述滤饼进行烘干、焙烧、破碎得到改性骨架空缺二氧化硅粉体；
5)将改性骨架空缺二氧化硅粉体、硅溶胶粘结剂混合后滚球成型、干燥、焙烧后制得。
4.根据权利要求3所述的制备方法，其特征在于，步骤1)所述硅酸钠中二氧化硅浓度为5-25wt％；所述无机酸为硫酸、盐酸、硝酸、磷酸中至少一种，无机酸浓度为5-30wt％；所述铝盐为硫酸铝、硝酸铝、异丙醇铝、偏铝酸钠中至少一种，铝盐或硼酸的添加量摩尔比为Al2O3或B2O3:SiO2＝(0.5-2):10。
5.根据权利要求3所述的制备方法，其特征在于，步骤2)所述有机-无机复合酸为0.5-5wt％，有机酸为乙酸、丙酸中一种，无机酸为盐酸、硝酸、硫酸、磷酸中一种，质量比有机酸：无机酸＝(0.1-5)：1。
6.根据权利要求3所述的制备方法，其特征在于，步骤3)所述金属盐水溶液浓度为0.05-0.5mol/L，金属盐水溶液与骨架空缺二氧化硅凝胶质量比为1:1。
7.根据权利要求3所述的制备方法，其特征在于，步骤4)所述二氧化硅粉体粒径目数为120-500目。
8.根据权利要求3所述的制备方法，其特征在于，步骤5)所述滚球成型吸附剂等效球直径尺寸为0.3-1.5mm。
9.一种权利要求1所述的吸附剂在脱除费托合成油含氧化合物的应用，其特征在于，所述的含氧化合物包括醇类、酸类、酯类、醛类、酮类，脱除前质量百分含量为0.1-10％，脱除后，费托合成油中含氧化合物质量分数降低至1ppm以下。
10.根据权利要求9所述的吸附剂在脱除费托合成油含氧化合物的应用，其特征在于，所述吸附剂应用于模拟移动床费托合成油脱氧工艺，模拟移动床吸附温度为50-150℃，吸附压力为0.1-2.0MPa，吸附塔床层数8-16层，解吸剂为烷烃和醇的混合物，吸附剂器内再生重复使用。
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