CN117504879A - 用于重油残渣、高粘油加氢改质的催化剂 - Google Patents
用于重油残渣、高粘油加氢改质的催化剂 Download PDFInfo
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- CN117504879A CN117504879A CN202210889833.2A CN202210889833A CN117504879A CN 117504879 A CN117504879 A CN 117504879A CN 202210889833 A CN202210889833 A CN 202210889833A CN 117504879 A CN117504879 A CN 117504879A
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- catalyst
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- oxide
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- 238000003756 stirring Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- YOUIDGQAIILFBW-UHFFFAOYSA-J tetrachlorotungsten Chemical compound Cl[W](Cl)(Cl)Cl YOUIDGQAIILFBW-UHFFFAOYSA-J 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical compound [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 2
- 150000003623 transition metal compounds Chemical class 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- DZKDPOPGYFUOGI-UHFFFAOYSA-N tungsten(iv) oxide Chemical compound O=[W]=O DZKDPOPGYFUOGI-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 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
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 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 description 2
- CGWDABYOHPEOAD-VIFPVBQESA-N (2r)-2-[(4-fluorophenoxy)methyl]oxirane Chemical compound C1=CC(F)=CC=C1OC[C@@H]1OC1 CGWDABYOHPEOAD-VIFPVBQESA-N 0.000 description 1
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 description 1
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
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- BHDYSZBQDHARMZ-UHFFFAOYSA-N B([S-])([O-])[O-].[Na+].[Na+].[Na+] Chemical compound B([S-])([O-])[O-].[Na+].[Na+].[Na+] BHDYSZBQDHARMZ-UHFFFAOYSA-N 0.000 description 1
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- 229910052684 Cerium Inorganic materials 0.000 description 1
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- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 1
- 229910021584 Cobalt(II) iodide Inorganic materials 0.000 description 1
- 229910021581 Cobalt(III) chloride Inorganic materials 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 1
- 239000005750 Copper hydroxide Substances 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
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- 239000004277 Ferrous carbonate Substances 0.000 description 1
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- 229910021579 Iron(II) iodide Inorganic materials 0.000 description 1
- 229910021576 Iron(III) bromide Inorganic materials 0.000 description 1
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- 241000408529 Libra Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- FQYLQLRMGOMEOK-UHFFFAOYSA-N [Mo+3]=O Chemical compound [Mo+3]=O FQYLQLRMGOMEOK-UHFFFAOYSA-N 0.000 description 1
- QDAYJHVWIRGGJM-UHFFFAOYSA-B [Mo+4].[Mo+4].[Mo+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O Chemical class [Mo+4].[Mo+4].[Mo+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QDAYJHVWIRGGJM-UHFFFAOYSA-B 0.000 description 1
- CZDHLVRPJMJXEX-UHFFFAOYSA-H [Mo+6].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O Chemical compound [Mo+6].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O CZDHLVRPJMJXEX-UHFFFAOYSA-H 0.000 description 1
- UTOOQUPDCAYZDH-UHFFFAOYSA-N [Mo+]=O Chemical compound [Mo+]=O UTOOQUPDCAYZDH-UHFFFAOYSA-N 0.000 description 1
- MNSISFIFZIXKGI-UHFFFAOYSA-N [Mo+]=S Chemical compound [Mo+]=S MNSISFIFZIXKGI-UHFFFAOYSA-N 0.000 description 1
- NWKACDZKWWORPZ-UHFFFAOYSA-N [N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[Ti+2] Chemical compound [N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[Ti+2] NWKACDZKWWORPZ-UHFFFAOYSA-N 0.000 description 1
- UCYXRZPFJJBQDL-UHFFFAOYSA-N acetic acid;molybdenum Chemical compound [Mo].[Mo].CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O UCYXRZPFJJBQDL-UHFFFAOYSA-N 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005377 adsorption chromatography Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- NKQIMNKPSDEDMO-UHFFFAOYSA-L barium bromide Chemical compound [Br-].[Br-].[Ba+2] NKQIMNKPSDEDMO-UHFFFAOYSA-L 0.000 description 1
- 229910001620 barium bromide Inorganic materials 0.000 description 1
- 150000001553 barium compounds Chemical class 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- SGUXGJPBTNFBAD-UHFFFAOYSA-L barium iodide Chemical compound [I-].[I-].[Ba+2] SGUXGJPBTNFBAD-UHFFFAOYSA-L 0.000 description 1
- 229940075444 barium iodide Drugs 0.000 description 1
- 229910001638 barium iodide Inorganic materials 0.000 description 1
- UXFOSWFWQAUFFZ-UHFFFAOYSA-L barium(2+);diformate Chemical compound [Ba+2].[O-]C=O.[O-]C=O UXFOSWFWQAUFFZ-UHFFFAOYSA-L 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- IELPSGPHQCRVQW-UHFFFAOYSA-L barium(2+);sulfanide Chemical compound [SH-].[SH-].[Ba+2] IELPSGPHQCRVQW-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 150000001622 bismuth compounds Chemical class 0.000 description 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- ILAHWRKJUDSMFH-UHFFFAOYSA-N boron tribromide Chemical compound BrB(Br)Br ILAHWRKJUDSMFH-UHFFFAOYSA-N 0.000 description 1
- YMEKEHSRPZAOGO-UHFFFAOYSA-N boron triiodide Chemical compound IB(I)I YMEKEHSRPZAOGO-UHFFFAOYSA-N 0.000 description 1
- ZOAIGCHJWKDIPJ-UHFFFAOYSA-M caesium acetate Chemical compound [Cs+].CC([O-])=O ZOAIGCHJWKDIPJ-UHFFFAOYSA-M 0.000 description 1
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 description 1
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 1
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 description 1
- KOPBYBDAPCDYFK-UHFFFAOYSA-N caesium oxide Chemical compound [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 1
- 229910001942 caesium oxide Inorganic materials 0.000 description 1
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- XQTIWNLDFPPCIU-UHFFFAOYSA-N cerium(3+) Chemical compound [Ce+3] XQTIWNLDFPPCIU-UHFFFAOYSA-N 0.000 description 1
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 description 1
- TYAVIWGEVOBWDZ-UHFFFAOYSA-K cerium(3+);phosphate Chemical compound [Ce+3].[O-]P([O-])([O-])=O TYAVIWGEVOBWDZ-UHFFFAOYSA-K 0.000 description 1
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 description 1
- KHSBAWXKALEJFR-UHFFFAOYSA-H cerium(3+);tricarbonate;hydrate Chemical compound O.[Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O KHSBAWXKALEJFR-UHFFFAOYSA-H 0.000 description 1
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 1
- MMXSKTNPRXHINM-UHFFFAOYSA-N cerium(3+);trisulfide Chemical compound [S-2].[S-2].[S-2].[Ce+3].[Ce+3] MMXSKTNPRXHINM-UHFFFAOYSA-N 0.000 description 1
- VZDYWEUILIUIDF-UHFFFAOYSA-J cerium(4+);disulfate Chemical compound [Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VZDYWEUILIUIDF-UHFFFAOYSA-J 0.000 description 1
- 229910000421 cerium(III) oxide Inorganic materials 0.000 description 1
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 229910000355 cerium(IV) sulfate Inorganic materials 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- UBFMILMLANTYEU-UHFFFAOYSA-H chromium(3+);oxalate Chemical compound [Cr+3].[Cr+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O UBFMILMLANTYEU-UHFFFAOYSA-H 0.000 description 1
- 229910000151 chromium(III) phosphate Inorganic materials 0.000 description 1
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 1
- IKZBVTPSNGOVRJ-UHFFFAOYSA-K chromium(iii) phosphate Chemical compound [Cr+3].[O-]P([O-])([O-])=O IKZBVTPSNGOVRJ-UHFFFAOYSA-K 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001869 cobalt compounds Chemical class 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 description 1
- AVWLPUQJODERGA-UHFFFAOYSA-L cobalt(2+);diiodide Chemical compound [Co+2].[I-].[I-] AVWLPUQJODERGA-UHFFFAOYSA-L 0.000 description 1
- XTUHPOUJWWTMNC-UHFFFAOYSA-N cobalt(2+);dioxido(dioxo)chromium Chemical compound [Co+2].[O-][Cr]([O-])(=O)=O XTUHPOUJWWTMNC-UHFFFAOYSA-N 0.000 description 1
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 description 1
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 description 1
- OOMOMODKLPLOKW-UHFFFAOYSA-H cobalt(3+);trisulfate Chemical compound [Co+3].[Co+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OOMOMODKLPLOKW-UHFFFAOYSA-H 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 229910000362 cobalt(III) sulfate Inorganic materials 0.000 description 1
- BZRRQSJJPUGBAA-UHFFFAOYSA-L cobalt(ii) bromide Chemical compound Br[Co]Br BZRRQSJJPUGBAA-UHFFFAOYSA-L 0.000 description 1
- YCYBZKSMUPTWEE-UHFFFAOYSA-L cobalt(ii) fluoride Chemical compound F[Co]F YCYBZKSMUPTWEE-UHFFFAOYSA-L 0.000 description 1
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 1
- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 description 1
- FCEOGYWNOSBEPV-FDGPNNRMSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FCEOGYWNOSBEPV-FDGPNNRMSA-N 0.000 description 1
- JUPWRUDTZGBNEX-UHFFFAOYSA-N cobalt;pentane-2,4-dione Chemical compound [Co].CC(=O)CC(C)=O.CC(=O)CC(C)=O.CC(=O)CC(C)=O JUPWRUDTZGBNEX-UHFFFAOYSA-N 0.000 description 1
- 229940116318 copper carbonate Drugs 0.000 description 1
- JGDFBJMWFLXCLJ-UHFFFAOYSA-N copper chromite Chemical compound [Cu]=O.[Cu]=O.O=[Cr]O[Cr]=O JGDFBJMWFLXCLJ-UHFFFAOYSA-N 0.000 description 1
- 150000004699 copper complex Chemical class 0.000 description 1
- 150000001880 copper compounds Chemical class 0.000 description 1
- 229910001956 copper hydroxide Inorganic materials 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- AWSWAKKAIQTOLD-UHFFFAOYSA-L copper;2,3-dihydroxypropanoate Chemical compound [Cu+2].OCC(O)C([O-])=O.OCC(O)C([O-])=O AWSWAKKAIQTOLD-UHFFFAOYSA-L 0.000 description 1
- ZKXWKVVCCTZOLD-UHFFFAOYSA-N copper;4-hydroxypent-3-en-2-one Chemical compound [Cu].CC(O)=CC(C)=O.CC(O)=CC(C)=O ZKXWKVVCCTZOLD-UHFFFAOYSA-N 0.000 description 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 1
- XNEQAVYOCNWYNZ-UHFFFAOYSA-L copper;dinitrite Chemical compound [Cu+2].[O-]N=O.[O-]N=O XNEQAVYOCNWYNZ-UHFFFAOYSA-L 0.000 description 1
- PWGQHOJABIQOOS-UHFFFAOYSA-N copper;dioxido(dioxo)chromium Chemical compound [Cu+2].[O-][Cr]([O-])(=O)=O PWGQHOJABIQOOS-UHFFFAOYSA-N 0.000 description 1
- IQKQUSLYXMWMQZ-UHFFFAOYSA-N copper;oxido-(oxido(dioxo)chromio)oxy-dioxochromium Chemical compound [Cu+2].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O IQKQUSLYXMWMQZ-UHFFFAOYSA-N 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- FZYODJBJGPYBCX-UHFFFAOYSA-N dibismuth;oxido-(oxido(dioxo)chromio)oxy-dioxochromium Chemical compound [Bi+3].[Bi+3].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O.[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O.[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O FZYODJBJGPYBCX-UHFFFAOYSA-N 0.000 description 1
- FWIZHMQARNODNX-UHFFFAOYSA-L dibismuth;oxygen(2-);carbonate Chemical compound [O-2].[O-2].[Bi+3].[Bi+3].[O-]C([O-])=O FWIZHMQARNODNX-UHFFFAOYSA-L 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- RJYMRRJVDRJMJW-UHFFFAOYSA-L dibromomanganese Chemical compound Br[Mn]Br RJYMRRJVDRJMJW-UHFFFAOYSA-L 0.000 description 1
- LSALTGRCOGBBFR-UHFFFAOYSA-L dibromotungsten Chemical compound Br[W]Br LSALTGRCOGBBFR-UHFFFAOYSA-L 0.000 description 1
- HEQUOWMMDQTGCX-UHFFFAOYSA-L dicesium;oxalate Chemical compound [Cs+].[Cs+].[O-]C(=O)C([O-])=O HEQUOWMMDQTGCX-UHFFFAOYSA-L 0.000 description 1
- QTNDMWXOEPGHBT-UHFFFAOYSA-N dicesium;sulfide Chemical compound [S-2].[Cs+].[Cs+] QTNDMWXOEPGHBT-UHFFFAOYSA-N 0.000 description 1
- UDJQAOMQLIIJIE-UHFFFAOYSA-L dichlorotungsten Chemical compound Cl[W]Cl UDJQAOMQLIIJIE-UHFFFAOYSA-L 0.000 description 1
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 description 1
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- MSNWSDPPULHLDL-UHFFFAOYSA-K ferric hydroxide Chemical compound [OH-].[OH-].[OH-].[Fe+3] MSNWSDPPULHLDL-UHFFFAOYSA-K 0.000 description 1
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 description 1
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 description 1
- 235000019268 ferrous carbonate Nutrition 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
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- 238000009499 grossing Methods 0.000 description 1
- OQVJXQJWYQNWTI-UHFFFAOYSA-H hexabromotungsten Chemical compound Br[W](Br)(Br)(Br)(Br)Br OQVJXQJWYQNWTI-UHFFFAOYSA-H 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- AQBLLJNPHDIAPN-LNTINUHCSA-K iron(3+);(z)-4-oxopent-2-en-2-olate Chemical compound [Fe+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O AQBLLJNPHDIAPN-LNTINUHCSA-K 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 229910000015 iron(II) carbonate Inorganic materials 0.000 description 1
- 229910000155 iron(II) phosphate Inorganic materials 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- LNOZJRCUHSPCDZ-UHFFFAOYSA-L iron(ii) acetate Chemical compound [Fe+2].CC([O-])=O.CC([O-])=O LNOZJRCUHSPCDZ-UHFFFAOYSA-L 0.000 description 1
- GYCHYNMREWYSKH-UHFFFAOYSA-L iron(ii) bromide Chemical compound [Fe+2].[Br-].[Br-] GYCHYNMREWYSKH-UHFFFAOYSA-L 0.000 description 1
- FZGIHSNZYGFUGM-UHFFFAOYSA-L iron(ii) fluoride Chemical compound [F-].[F-].[Fe+2] FZGIHSNZYGFUGM-UHFFFAOYSA-L 0.000 description 1
- BQZGVMWPHXIKEQ-UHFFFAOYSA-L iron(ii) iodide Chemical compound [Fe+2].[I-].[I-] BQZGVMWPHXIKEQ-UHFFFAOYSA-L 0.000 description 1
- SDEKDNPYZOERBP-UHFFFAOYSA-H iron(ii) phosphate Chemical compound [Fe+2].[Fe+2].[Fe+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SDEKDNPYZOERBP-UHFFFAOYSA-H 0.000 description 1
- SHXXPRJOPFJRHA-UHFFFAOYSA-K iron(iii) fluoride Chemical compound F[Fe](F)F SHXXPRJOPFJRHA-UHFFFAOYSA-K 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical group 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
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- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229960001708 magnesium carbonate Drugs 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 150000002681 magnesium compounds Chemical class 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- UHNWOJJPXCYKCG-UHFFFAOYSA-L magnesium oxalate Chemical compound [Mg+2].[O-]C(=O)C([O-])=O UHNWOJJPXCYKCG-UHFFFAOYSA-L 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- AAJBNRZDTJPMTJ-UHFFFAOYSA-L magnesium;dinitrite Chemical compound [Mg+2].[O-]N=O.[O-]N=O AAJBNRZDTJPMTJ-UHFFFAOYSA-L 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 235000006748 manganese carbonate Nutrition 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 150000002697 manganese compounds Chemical class 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 description 1
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 description 1
- OYMJNIHGVDEDFX-UHFFFAOYSA-J molybdenum tetrachloride Chemical compound Cl[Mo](Cl)(Cl)Cl OYMJNIHGVDEDFX-UHFFFAOYSA-J 0.000 description 1
- ZSSVQAGPXAAOPV-UHFFFAOYSA-K molybdenum trichloride Chemical compound Cl[Mo](Cl)Cl ZSSVQAGPXAAOPV-UHFFFAOYSA-K 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- BQBYSLAFGRVJME-UHFFFAOYSA-L molybdenum(2+);dichloride Chemical compound Cl[Mo]Cl BQBYSLAFGRVJME-UHFFFAOYSA-L 0.000 description 1
- GMMJTCLAKDKBCZ-UHFFFAOYSA-L molybdenum(ii) bromide Chemical compound Br[Mo]Br GMMJTCLAKDKBCZ-UHFFFAOYSA-L 0.000 description 1
- AQRDGTBNWBTFKJ-UHFFFAOYSA-N molybdenum;dihydrate Chemical compound O.O.[Mo] AQRDGTBNWBTFKJ-UHFFFAOYSA-N 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
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- 150000002816 nickel compounds Chemical class 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910000159 nickel phosphate Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 description 1
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 description 1
- JOCJYBPHESYFOK-UHFFFAOYSA-K nickel(3+);phosphate Chemical compound [Ni+3].[O-]P([O-])([O-])=O JOCJYBPHESYFOK-UHFFFAOYSA-K 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- FYFRKQBKFGRDSO-UHFFFAOYSA-H oxalate;titanium(3+) Chemical compound [Ti+3].[Ti+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O FYFRKQBKFGRDSO-UHFFFAOYSA-H 0.000 description 1
- DAWBXZHBYOYVLB-UHFFFAOYSA-J oxalate;zirconium(4+) Chemical compound [Zr+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O DAWBXZHBYOYVLB-UHFFFAOYSA-J 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- BDVMTRCCIQHRBL-UHFFFAOYSA-J phosphonato phosphate;titanium(4+) Chemical compound [Ti+4].[O-]P([O-])(=O)OP([O-])([O-])=O BDVMTRCCIQHRBL-UHFFFAOYSA-J 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 150000003112 potassium compounds Chemical class 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
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- KAQHZJVQFBJKCK-UHFFFAOYSA-L potassium pyrosulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OS([O-])(=O)=O KAQHZJVQFBJKCK-UHFFFAOYSA-L 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- WXBOMIKEWRRKBB-UHFFFAOYSA-N rhenium(iv) oxide Chemical compound O=[Re]=O WXBOMIKEWRRKBB-UHFFFAOYSA-N 0.000 description 1
- USBWXQYIYZPMMN-UHFFFAOYSA-N rhenium;heptasulfide Chemical compound [S-2].[S-2].[S-2].[S-2].[S-2].[S-2].[S-2].[Re].[Re] USBWXQYIYZPMMN-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical compound O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 150000003388 sodium compounds Chemical class 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- ZVTQDOIPKNCMAR-UHFFFAOYSA-N sulfanylidene(sulfanylideneboranylsulfanyl)borane Chemical compound S=BSB=S ZVTQDOIPKNCMAR-UHFFFAOYSA-N 0.000 description 1
- PTISTKLWEJDJID-UHFFFAOYSA-N sulfanylidenemolybdenum Chemical compound [Mo]=S PTISTKLWEJDJID-UHFFFAOYSA-N 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- WWJBJTBTXOHQAZ-UHFFFAOYSA-J tetrabromomolybdenum Chemical compound Br[Mo](Br)(Br)Br WWJBJTBTXOHQAZ-UHFFFAOYSA-J 0.000 description 1
- KXLQKNLVPVYVKX-UHFFFAOYSA-J tetrabromorhenium Chemical compound Br[Re](Br)(Br)Br KXLQKNLVPVYVKX-UHFFFAOYSA-J 0.000 description 1
- UXMRNSHDSCDMLG-UHFFFAOYSA-J tetrachlororhenium Chemical compound Cl[Re](Cl)(Cl)Cl UXMRNSHDSCDMLG-UHFFFAOYSA-J 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- ALRFTTOJSPMYSY-UHFFFAOYSA-N tin disulfide Chemical compound S=[Sn]=S ALRFTTOJSPMYSY-UHFFFAOYSA-N 0.000 description 1
- FBGKGORFGWHADY-UHFFFAOYSA-L tin(2+);dihydroxide Chemical compound O[Sn]O FBGKGORFGWHADY-UHFFFAOYSA-L 0.000 description 1
- OBBXFSIWZVFYJR-UHFFFAOYSA-L tin(2+);sulfate Chemical compound [Sn+2].[O-]S([O-])(=O)=O OBBXFSIWZVFYJR-UHFFFAOYSA-L 0.000 description 1
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 description 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 1
- 229910021509 tin(II) hydroxide Inorganic materials 0.000 description 1
- 229910000375 tin(II) sulfate Inorganic materials 0.000 description 1
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- UBZYKBZMAMTNKW-UHFFFAOYSA-J titanium tetrabromide Chemical compound Br[Ti](Br)(Br)Br UBZYKBZMAMTNKW-UHFFFAOYSA-J 0.000 description 1
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 1
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 description 1
- SOBXOQKKUVQETK-UHFFFAOYSA-H titanium(3+);trisulfate Chemical compound [Ti+3].[Ti+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O SOBXOQKKUVQETK-UHFFFAOYSA-H 0.000 description 1
- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-UHFFFAOYSA-N 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 1
- NLPMQGKZYAYAFE-UHFFFAOYSA-K titanium(iii) fluoride Chemical compound F[Ti](F)F NLPMQGKZYAYAFE-UHFFFAOYSA-K 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- FEONEKOZSGPOFN-UHFFFAOYSA-K tribromoiron Chemical compound Br[Fe](Br)Br FEONEKOZSGPOFN-UHFFFAOYSA-K 0.000 description 1
- YPFBRNLUIFQCQL-UHFFFAOYSA-K tribromomolybdenum Chemical compound Br[Mo](Br)Br YPFBRNLUIFQCQL-UHFFFAOYSA-K 0.000 description 1
- IEKWPPTXWFKANS-UHFFFAOYSA-K trichlorocobalt Chemical compound Cl[Co](Cl)Cl IEKWPPTXWFKANS-UHFFFAOYSA-K 0.000 description 1
- KOECRLKKXSXCPB-UHFFFAOYSA-K triiodobismuthane Chemical compound I[Bi](I)I KOECRLKKXSXCPB-UHFFFAOYSA-K 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 description 1
- FZFRVZDLZISPFJ-UHFFFAOYSA-N tungsten(6+) Chemical compound [W+6] FZFRVZDLZISPFJ-UHFFFAOYSA-N 0.000 description 1
- UXVOMHPBSSIGNQ-UHFFFAOYSA-I tungsten(v) bromide Chemical compound Br[W](Br)(Br)(Br)Br UXVOMHPBSSIGNQ-UHFFFAOYSA-I 0.000 description 1
- WIDQNNDDTXUPAN-UHFFFAOYSA-I tungsten(v) chloride Chemical compound Cl[W](Cl)(Cl)(Cl)Cl WIDQNNDDTXUPAN-UHFFFAOYSA-I 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- JQOAZIZLIIOXEW-UHFFFAOYSA-N zinc;chromium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Cr+3].[Cr+3].[Zn+2] JQOAZIZLIIOXEW-UHFFFAOYSA-N 0.000 description 1
- NDKWCCLKSWNDBG-UHFFFAOYSA-N zinc;dioxido(dioxo)chromium Chemical compound [Zn+2].[O-][Cr]([O-])(=O)=O NDKWCCLKSWNDBG-UHFFFAOYSA-N 0.000 description 1
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 description 1
- KHADWTWCQJVOQO-UHFFFAOYSA-N zinc;oxido-(oxido(dioxo)chromio)oxy-dioxochromium Chemical compound [Zn+2].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KHADWTWCQJVOQO-UHFFFAOYSA-N 0.000 description 1
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 description 1
- 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 description 1
- LSWWNKUULMMMIL-UHFFFAOYSA-J zirconium(iv) bromide Chemical compound Br[Zr](Br)(Br)Br LSWWNKUULMMMIL-UHFFFAOYSA-J 0.000 description 1
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Abstract
本发明提供了用于重油残渣、高粘油加氢改质的催化剂,涉及催化剂技术领域,该催化剂由多孔载体、二级载体和活性成分构成,还可加入修饰元素,具有较优的活性、使用周期、传质效果,能够提高加氢改质的效率,能够有效应用于重油残渣、高粘油的加氢改质。
Description
技术领域
本发明涉及催化剂技术领域,具体涉及用于重油残渣、高粘油加氢改质的催化剂。
背景技术
已知催化剂(俄罗斯联邦专利第2414297号“不规则、非球形载体上的催化剂和重质石油馏分的加氢转化方法”,IPC B01J21/04、B01J23/40、B01J23/24、B01J23/74、B01J302、B01J35/10、C10G47/10、C10G45/04,优先权日期12/14/2006,发布于03/20/2011)用于重烃的加氢改质。该催化剂载体为氧化铝、催化金属为VIB和VIII族催化金属的一种或者化合物,其多孔结构由多个连续的团块组成,每个团块由多个针状板形成。通常,每个团块的板相对于另一个团块中心呈径向分布。上述骨架具有不规则和非球形形状,且大多为氧化铝球破碎后的碎片形式。载体制备方法如下:a)从结晶性差的活性氧化铝粉末开始造粒,以获得珠状的团聚体;b)在60℃至100℃温度范围内的潮湿环境中熟化,然后干燥上述团聚体;c)筛分并回收上述团聚体;d)粉碎上述部分;f)在250℃至900℃的温度范围内煅烧上述粉碎部分;f)在80℃至250℃的温度范围内进行酸浸和水热处理;g)干燥,然后在500℃至1100℃的温度范围内煅烧。得到的催化剂在用于重烃的改质处理时表现出更好的性能。这种催化剂的缺点是它的制备过程是多阶段的。
已知催化剂(俄罗斯联邦专利号2607908“碳氢化合物原料加氢改质催化剂的制备方法”,IPC B01J 37/02、B01J 38/62、B01J 20/16、B01J 23/883、C10G 47/12,优先权日期2015年11月5日,2017年1月11日出版)。催化剂含有镍、钼、铝和硅。该方法包括制备含有质量分数50-80%氧化铝颗粒的载体,Si/Al质量比为0.6至0.85的非晶态铝硅酸盐,使用双金属络合物[Ni(Н2O)x(L)y]2[Мо4O11(С6Н5O7)2],其中L是柠檬酸С6Н5О7的部分脱质子形式;x=0或2;y=0或1,催化剂在100-250℃温度下干燥,所得催化剂中组分的质量百分比如下:[Ni(Н2O)x(L)y]2[Мо4O11(С6Н5O7)2]–13.1-23.3;非晶硅铝酸盐–40.0-61.3;γ-Al2O3-其余部分。在550℃下煅烧所得催化剂中组分的质量百分比如下:MoO3–7.0-13.0;NiO–1.8-3.4;非晶硅铝酸盐–43,1-66,9;γ-Al2O3–其余部分。在加氢改质中使用了以这种方式制备的催化剂,可以提高柴油馏分的产量。这种催化剂的缺点是活性低。
已知催化剂(俄罗斯联邦专利号2506997“处理重油馏分的催化剂”,IPC B01J23/74、B01J23/24、B01J35/10、B82B1/00、C10G45/00,优先权日期为2012年8月27日,于2014年2月20日发布。)。在催化剂中,活性组分选自镍、钴、钼、钨或其组合的化合物。载体由氧化铝、二氧化硅、钛、锆、铝硅酸盐、硅酸铁或其组合的无机多孔载体。所述催化剂含有规则的大孔结构,大于50nm的大孔占所述催化剂总孔体积的至少30%。该催化剂活性不足,由于低扩散特性而导致传质值低和使用周期短。
专利号为CN201310428555.1的中国专利“一种用于稠油改质降粘用超分散催化剂的制备方法及其应用”,其特征在于,按质量份数计,所需的原料为:基础油150~200、表面活性剂5~15、过渡金属化合物1.5~2、助表面活性剂1~1.5;将上述所述原料在40~80℃温度下进行混合,控制在100~8000转/分搅拌5~300min后,控制超声频率在10~50KHz范围内,经超声震荡10~30min,得到纳米级反胶束微乳液,即所需的用于稠油改质降粘用超分散催化剂。该催化剂不具有高孔隙度结构载体,催化剂活性较低。
专利号为CN201810015975.X的中国专利“一种稠油改质催化剂及其制备方法”,所述蛋壳粉通过如下步骤制备得到:将清洗并干燥后的蛋壳进行煅烧,冷却后进行研磨,得到蛋壳粉;所述溶剂载体为稠油、常压渣油、减压渣油和沥青中任一种。本发明使用的蛋壳具有来源广且不受地理位置限制的优点;本发明能够有效利用废弃资源,减少环境污染。该催化剂扩散特性差,使用周期短。
专利号为CN202110505117.5的中国专利“一种稠油改质镍基催化剂及其制备方法和应用”,所述镍基催化剂包括载体,所述载体表面负载有活性组分;所述载体为金属氧化物;所述金属氧化物具有通式:A(1x)BxO2,其中,A选自过渡金属元素,B选自镧系元素;所述活性组分至少包括Ni。本发明的技术路线无需其他添加剂,在较短时间、较低温度和压力下实现了降粘的目的,操作方便,适合于规模化工业应用,但活性组分有限制,而且报道的催化效果差(从降粘率来看)。
专利号为CN201310428555.1的中国专利“一种用于稠油改质降粘用超分散催化剂的制备方法及其应用”,其特征在于,按质量份数计,所需的原料为:基础油150~200、表面活性剂5~15、过渡金属化合物1.5~2、助表面活性剂1~1.5;将上述所述原料在40~80℃温度下进行混合,控制在100~8000转/分搅拌5~300min后,控制超声频率在10~50KHz范围内,经超声震荡10~30min,得到纳米级反胶束微乳液,即所需的用于稠油改质降粘用超分散催化剂。该催化剂不具有高孔隙度结构载体,催化剂活性较低。
专利号为CN201810015975.X的中国专利“一种稠油改质催化剂及其制备方法”,所述蛋壳粉通过如下步骤制备得到:将清洗并干燥后的蛋壳进行煅烧,冷却后进行研磨,得到蛋壳粉;所述溶剂载体为稠油、常压渣油、减压渣油和沥青中任一种。本发明使用的蛋壳具有来源广且不受地理位置限制的优点;本发明能够有效利用废弃资源,减少环境污染。该催化剂扩散特性差,使用周期短。
针对现有技术中催化剂存在的各类问题,寻找一种具有较优的活性、使用周期以及传质效果,能够用于重油残渣、高粘油加氢改质十分必要。
发明内容
本发明针对现有技术存在的问题,提供了用于重油残渣、高粘油加氢改质的催化剂,该催化剂能够提高催化剂的活性,延长催化剂的使用周期,提高改质过程中的传质效率,提高改质效率。
本发明提供了一种催化剂,包括无机多孔载体、二级载体和活性成分;所述二级载体的原料包括沸石、氧化铝、氧化铁、氧化硅、氧化钛、氧化锆、硅酸铝、硅酸铁和粘土中的一种或多种。
进一步地,所述无机多孔载体的起始金属包括镍、铬、铜、铁、钛、铝、氧化铝和氧化铁中的一种或多种。
进一步地,所述无机多孔载体的孔隙率在85%以上,平均孔径为0.5-6.0mm。
进一步地,二级载体厚度为10微米至2000微米,比表面积大于20m2/g,孔体积为0.1至1.0cm3/g,其中直径大于5nm的孔占总孔体积大于50%;
进一步地,二级载体存在Bronsted和Lewis酸位,Bronsted和Lewis中氨的升温脱附温度为250-350℃和350℃以上,强酸位的数量分别为1-1500和1-1500μmol/g,Bronsted和Lewis的中酸性和强酸位置比例为1.10:1.5
进一步地,所述二级载体固定在无机多孔载体上,所述活性成分固定在二级载体上。
进一步地,所述的催化剂按重量百分比计,包括:5-40%二级载体和0.05-40%活性成分和余量无机多孔载体。
进一步地,所述活性成分包括:镍、钴、钼或钨的化合物中的一种或多种。
进一步地,所述催化剂还包括修饰元素。
进一步地,所述修饰元素包括K、Na、Mg、Zn、Cu、Re、Bi、Mn、Ba、Sn、B、Ce、Cs、Fe、Cr、Ti、Zr、Si和稀土元素中的一种或多种。
本发明还提供了上述催化剂的制备方法,包括以下步骤:
S1:无机多孔载体的制备:将金属通过电化学沉积法或滑移法制得;
S2:向无机多孔载体中加入含有二级载体初始元素的溶液中,浸渍,干燥和/或煅烧,得到物料A;
S3:将物料A置于含有活性成分的水溶液中,加热浸渍,再次加热去除溶剂,干燥、煅烧、还原,即得催化剂。
在另外一些实施方式中,上述催化剂的制备方法,包括以下步骤:
(1)无机多孔载体的制备:将金属通过电化学沉积法或滑移法制得;
(2)向无机多孔载体中加入含有二级载体初始元素的溶液中,浸渍,干燥和/或煅烧,得到物料A;
(3)将物料A浸渍在含有修饰元素的化合物的水溶液中;加热去除溶剂,干燥,煅烧;得到物料B;
(4)将物料B置于含有活性成分的水溶液中,加热浸渍,再次加热去除溶剂,干燥、煅烧、还原,即得催化剂。
进一步地,本发明通过将金属电化学沉积或通过滑移法获得无机多孔载体(也称高度多孔载体)。
电化学沉积:金属在网状多孔聚氨酯泡沫基质的金属化基材上的电化学沉积分三个阶段进行:在聚氨酯泡沫基质上施加导电层;金属涂层在金属化聚氨酯泡沫基质上的电化学沉积;和在300-1900℃的温度下煅烧2-8小时去除有机聚氨酯泡沫基质。
滑移法:将金属粉末应用于网状多孔聚氨酯泡沫基质并进行循环作用(压缩-拉伸)复制聚氨酯泡沫基质。然后将样品挤压到给定的重量去除多余的滑移物。再将浸渍过的工件依次在100-120℃的温度下干燥1-4小时,并在1200-1900℃温度下退火2-8小时。
其中,金属载体具体为:镍、铬、铜、铁、钛、铝以单独形式或彼此组合用作无机多孔载体的起始金属。
进一步地,本发明通过滑移法获得由氧化铝、氧化铁或彼此组合制成的无机多孔载体,该方法包括通过循环作用(压缩-张力)用铝化合物溶液浸渍多孔聚氨酯泡沫基体。然后,通过将样品挤压到给定的重量来去除多余的滑移物。然后将浸渍过的工件依次在100-120℃的温度下干燥1-4小时,并在1200-1700℃的温度下退火2-8小时。同时,氧化铝的各种变体(γ-Al2O3、β-Al2O3、η-Al2O3、δ-Al2O3、θ-Al2O3、α-Al2O3),形成单独形式或彼此组合的氧化物。
各种盐、氢氧化物和氧化铝用作起始化合物,以获得单独形式或彼此组合的高度多孔氧化铝载体。
使用单独形式或彼此组合的各种盐、氢氧化物和氧化铁作为起始化合物以获得高度多孔的氧化铁载体。
同时,在采用滑移法从金属、氧化铝或氧化铁中获得载体时,为了增加滑移液固定在网状网孔聚氨酯泡沫基体表面时的沉降稳定性和粘附强度,可以将表面活性剂溶液加入到滑移液中。
进一步地,为了形成沸石、氧化铝、氧化硅、氧化钛、氧化锆、铝硅酸盐、硅酸铁、氧化铁、粘土或其任何组合的二层载体,高度多孔金属、氧化铝或氧化铁载体的表面需要用这些元素的化合物浸渍。为此,将无机多孔载体的样品置于混合室中。然后,加入含有这些元素的初始化合物的水溶液或有机溶液。在20-80℃的温度下,用元素化合物溶液浸渍高度多孔的载体0.1-2小时。浸渍后,将高度多孔的载体在30-250℃的温度下干燥0.5-2小时。用于构成第二层载体沸石、氧化铝、氧化硅、氧化钛、氧化锆、铝硅酸盐、硅酸铁、氧化铁、粘土或其任意组合的总质量分数大于5%。由金属或元素的氧化铝化合物对无机多孔载体的总催化剂物质浸渍进行一次或多次,并在每次浸渍后干燥和/或煅烧。同时,当在高度多孔的多孔材料的表面上获得沸石、氧化铝、氧化硅、氧化钛、氧化锆、铝硅酸盐、硅酸铁、氧化铁、粘土或其任意组合的第二层时,以增加将铝化合物固定在由金属和氧化铝制成的多孔载体表面时的沉降稳定性和粘合强度,可以将表面活性剂溶液加入元素化合物的水溶液中。然后,为了将沉积的元素化合物转化为氧化物形式,多孔载体与元素化合物一起煅烧。在250℃至1200℃的温度下将具有施加的元素化合物的载体煅烧2-8小时以形成沸石、氧化铝、氧化硅、氧化钛、氧化锆、铝硅酸盐、硅酸铁、氧化铁、粘土或它们的任何组合,单独或相互组合。氧化铝二级载体的特征是厚度为10微米至2000微米,比表面积至少为20m2/g,孔体积为0.1至1.0cm3/g,孔径大于5nm,至少占总孔体积的50%。催化剂总组合物中的二层载体氧化铝至少为质量的5%。使用一层厚度至少为10微米以上,二次氧化铝层质量至少为总质量的5%,是由于需要形成一定量的活性相进行转化粘性油、重油和超重油残渣。
进一步地,选自镍、钴、钼、钨或其任意组合的化合物的活性成分的引入在将辅助载体固定在高度多孔的多孔载体上和/或通过用浸渍高度多孔的多孔载体的阶段进行。附加的辅助支撑。应用活性组分的化合物后,将催化剂在50℃至250℃的温度下干燥1-2小时,并在250℃至800℃的温度下煅烧2-8小时。
进一步地,氢氧化镍、硝酸镍、硫酸镍、磷酸镍、氯化镍、碳酸镍、草酸镍、乙酸镍、乙酰丙酮镍、单独形式或彼此组合的镍的有机金属络合物用作起始镍化合物。
进一步地,作为初始钴化合物的来源:氧化钴(II)、氧化钴(II,III)、氧化钴(III)、氢氧化钴、氟化钴(II)、溴化钴(II)、氯化钴(II)、氯化钴(III)、碘化钴(II)、硝酸钴(II)、碳酸钴(II)、草酸钴(II)、醋酸钴(II)、乙酰丙酮钴(II)、乙酰丙酮钴(III)、铬酸钴(II),与含钴阴离子(例如,二硫酸钾、六硝基钴酸钠等)的络合物,单独或相互组合。
进一步地,作为初始钼化合物的来源:氧化钼(III)、氧化钼(IV)、氧化钼(V)、氧化钼(VI)、氢氧化钼(III)、溴化钼(II)、溴化钼(III),溴化钼(IV),氯化钼(II),氯化钼(III),氯化钼(IV),氯化钼(V),硫化钼(II),硫化钼(III),硫化钼(IV),钼磷酸盐、钼酸、超钼酸、仲钼酸铵、草酸钼(VI)、乙酸钼(II)、二氧化钼(VI)(乙酰丙酮)、钼的有机金属络合物,单独或相互组合。
进一步地,作为初始钨化合物的来源:氧化钨(IV)、氧化钨(VI)、氟化钨(VI)、溴化钨(II)、溴化钨(V)、溴化钨(VI)、氯化钨(II)、氯化钨(IV)、氯化钨(V)、氯化钨(VI)、钨酸、草酸钨(V)、钨的有机金属络合物以单独形式或彼此组合使用。
进一步地,催化剂还可以包含额外的修饰元素。修饰元素是选自以下:K、Na、Mg、Zn、Cu、Re、Bi、Mn、Ba、Sn、B、Ce、Cs、Fe、Cr、Ti、Zr、Si、稀土元素至少一种或其任何组合。如有必要,在以下情况下引入修饰元素:在高孔隙度材料的合成阶段;对无机多孔载体施加浸渍;在将第二载体固定在高孔隙度材料的阶段;用固定的第二载体浸渍高孔隙度材料。
进一步地,应用修饰元素的化合物后,将催化剂在50℃至250℃的温度下干燥1-2小时,并在250℃至800℃的温度下煅烧2-8小时。
进一步地,氢氧化钾、硝酸钾、溴化钾、硫酸钾、硫酸钾、硫酸钾、碳酸钾、磷酸钾、氯化钾、草酸钾、钾的有机金属络合物以单独形式或彼此组合用作初始钾化合物。
进一步地,氢氧化钠、硝酸钠、溴化钠、连二亚硫酸钠、硫酸钠、硫酸钠、碳酸钠、磷酸钠、氯化钠、草酸钠、单独形式或彼此组合的有机金属钠络合物用作初始钠化合物。
进一步地,氢氧化镁、硝酸镁、亚硝酸镁、碳酸镁、磷酸镁、乙酸镁、草酸镁、镁的有机金属络合物以单独形式或彼此组合用作起始镁化合物。
进一步地,氢氧化锌、硫酸锌、硝酸锌、磷酸锌、氯化锌、碳酸锌、铬酸锌、重铬酸锌、亚铬酸锌、草酸锌、乙酸锌、乙酰丙酮锌、单独形式或彼此组合的有机金属锌络合物。
进一步地,硫酸铜、氢氧化铜、硝酸铜、亚硝酸铜、碳酸铜、亚铬酸铜、铬酸铜、重铬酸铜、醋酸铜、乙酰丙酮铜、铜与多元醇的络合物(例如,甘油酸铜等)或其混合物、有机金属单独形式或相互组合的铜络合物用作初始铜化合物。
进一步地,铼酸、氯化铼、溴化铼、硫化铼、高铼酸铵、氧化铼(IV)、氧化铼(VII)、铼的有机金属络合物以单独形式或彼此组合用作铼的起始化合物。
进一步地,硝酸铋、氢氧化铋、硫化铋、重铬酸铋、氢氧化铋、碘化铋、碳酸氧铋、氯氧化铋、铋的有机金属络合物以单独形式或彼此组合用作初始铋化合物。
进一步地,硝酸锰(II)、氯化锰(II)、溴化锰(II)、硫酸锰(II)、碳酸锰(II)、高锰酸锰、锰(II)的有机金属络合物,单独或相互组合用作初始锰化合物.
进一步地,氢氧化钡、硝酸钡、溴化钡、碘化钡、氢硫化钡、碳酸钡、硫酸钡、甲酸钡、钡的有机金属络合物以单独形式或彼此组合用作初始钡化合物。
进一步地,氧化锡(II)、氧化锡(IV)、氢氧化锡(II)、硫酸锡(II)、硫酸锡(IV)、氯化锡(II)、氯化锡(IV)、硫化锡(II)、锡(IV)硫化物、六氯锡酸氢(IV)、六羟基锡酸钠(IV)、单独形式或相互组合的锡的有机金属配合物用作初始锡化合物。
进一步地,氧化硼、三氢氧化硼、硼酸、氟化硼、溴化硼、碘化硼、硫化硼、氢氟酸、偏硼酸钠、四硼酸钠、四氟硼酸铵、四氟硼酸钠、四氢硼酸钠、硫代硼酸钠、三氟氨基硼、有机四氟硼酸钠、硼的单独形式或相互组合用作初始硼化合物。
进一步地,氧化铈(III)、氧化铈(IV)、硝酸铈(III)、硫酸铈(III)、硫酸铈(IV)、硫化铈(III)、碳酸铈(III)和磷酸铈用作初始铈化合物。(III)、草酸铈(III)、乙酸铈(III)、乙酰丙酮酸铈(III)、单独形式或彼此组合的铈的有机金属络合物用作初始铈化合物。
进一步地,氧化铯、氟化铯、氯化铯、溴化铯、碘化铯、硫化铯、硝酸铯、硫酸铯、草酸铯、乙酸铯、乙酰丙酮铯、铯的有机金属配合物,单独或与相互组合用作初始铯化合物。
进一步地,氧化铁(III)、氧化铁(II、III)、氢氧化铁(III)、硝酸铁(III)、硫酸铁(II)、硫酸钴(III)、磷酸铁(II)被用作初始铁化合物。、磷酸铁(III)、氟化铁(II)、氟化铁(III)、溴化铁(II)、溴化铁(III)、碘化铁(II)、氯化铁(II)、氯化铁(III)、碳酸盐铁(II)、草酸铁(II)、草酸铁(III)、乙酸铁(II)、乙酰丙酮酸铁(III),单独或相互组合用作初始铁化合物。
进一步地,硝酸铬、硫酸铬、磷酸铬、草酸铬、铬酸、铬酸钾、铬的有机金属络合物以单独形式或彼此组合用作初始铬化合物。
进一步地,氧化钛(III)、氧化钛(IV)、硝酸钛(II)、氟化钛(III)、氟化钛(IV)、氯化钛(II)、氯化钛(III)、氯化钛(IV)、钛(IV)溴化物、碘化钛(IV)、硫酸钛(III)、焦磷酸钛、草酸钛(III)、钛酸、单独形式或相互组合的有机金属钛络合物。
进一步地,氢氧化锆、氧化锆、硝酸锆、氟化锆、氯化锆、溴化锆、碘化锆、硫酸锆、草酸锆、单独形式或彼此组合的锆的有机金属络合物用作初始锆化合物。
进一步地,氧化硅、氢氧化硅、硅酸、硅钨酸、硅氟酸、有机硅化合物、单独形式或彼此组合的硅络合物用作初始硅化合物。
进一步地,蒸馏水、醋酸、硫酸、硝酸、高氯酸等酸的水溶液,二甲胺、三甲胺、丙胺、丁胺、甲苯、苯、乙腈、二氯甲烷、氨溶液、氯仿、丙酮作为溶剂用于起始应用修饰元素的化合物、羟胺、有机醚、醇或其混合物,以及其他溶剂。
为实现上述目的,本发明采用的技术方案如下:
本发明所取得的技术效果是:
本发明改善了催化剂的扩散特性,消除了起始化合物和反应产物运输传递过程中的扩散限制,抑制焦炭生成,消除了碳沉积物对孔隙的堵塞。该发明的另一项重要技术创新是提高了重油残渣、高粘度油、重油和超重油的加氢改质处理速率,油组分产率高,气相碳氢化合物的形成速率和产率低。这些技术创新将为目前催化改质存在的问题提供解决方案。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式,本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用,本说明书中的各项细节也可以基于不同观点与应用,在没有背离本发明的精神下进行各种修饰或改变。
在进一步描述本发明具体实施方式之前,应理解,本发明的保护范围不局限于下述特定的具体实施方案;还应当理解,本发明实施例中使用的术语是为了描述特定的具体实施方案,而不是为了限制本发明的保护范围。
当实施例给出数值范围时,应理解,除非本发明另有说明,每个数值范围的两个端点以及两个端点之间任何一个数值均可选用。除非另外定义,本文中使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同意义。
值得说明的是,本发明中使用的原料均为普通市售产品,因此对其来源不做具体限定。
载体合成:
在第一阶段,合成无机多孔载体。
通过两种方法获得无机多孔载体。第一种方法包括将金属电化学沉积在高度多孔的聚氨酯泡沫基质上。它是一种网状多孔聚氨酯泡沫基质。
金属在高度多孔聚氨酯泡沫基体上的电化学沉积分三个阶段进行:
①在高孔聚氨酯泡沫基质上沉积导电层;
②在金属化的高孔聚氨酯泡沫基体上电化学沉积金属;
③通过在300-1900℃的温度下煅烧2-8小时来去除有机聚氨酯泡沫基质。
通过在高度多孔的聚氨酯泡沫基质上施加金属粉末的悬浮液,通过光滑法施加金属。然后将过量的浆料去除至指定的质量。然后,我们依次在100-120℃下干燥具有金属粉末的高孔聚氨酯泡沫基质1-4小时,并在1200-1900℃下烧制2-8小时。
镍、铬、铜、铁、钛、铝以单独形式或组合形式作为载体的初始金属。
采用切片法制备氧化铝载体、氧化铁载体或组合,将铝或铁化合物悬浮液或它们的组合施加到高多孔聚氨酯泡沫基体表面。然后,将过量的浆料(金属化合物)去除。然后依次在100-120℃的温度下将具有金属化合物的高多孔聚氨酯泡沫基体干燥1-4小时,并在1200-1700℃的温度下烧制2-8小时。形成了各种形式的氧化铝(γ-Al2O3,β-Al2O3,η-Al2O3,δ-Al2O3,θ-Al2O3,α-Al2O3)、氧化铁以单独形式或相互组合。
各种盐、氢氧化物、氧化铝以单独形式或彼此组合用作初始化合物以获得高度多孔的氧化铝载体。
各种盐、氢氧化物、氧化铁以单独形式或彼此组合用作初始化合物以获得高度多孔的氧化铁载体。
当通过浆料法从金属、氧化铝或氧化铁制取多孔载体,从而增加沉降稳定性和粘合强度,同时将浆料固定在浆料水溶液中聚氨酯泡沫基质的表面上时,可以添加表面活性物质的溶液。
在第二阶段,在多孔载体的表面上形成第二载体层(二级载体)。
将多孔载体的表面浸渍有这些元素的化合物,从而形成沸石、氧化铝、氧化硅、氧化钛、氧化锆、铝硅酸盐、硅酸铁、氧化铁、粘土或它们的任意组合的第二层载体。首先,将多孔载体的样品置于混合室中。然后,投配初始元素化合物的水溶液或有机溶液或悬浮液。元素化合物的溶液或悬浮液在20-80℃温度下在0.1-2小时内施加到多孔介质表面。沸石、氧化铝、氧化硅、氧化钛、氧化锆、铝硅酸盐、硅酸铁、氧化铁、粘土或这些的任何组合的第二层施加到多孔材料的表面可以增加沉降稳定。当素化合物固定在高度多孔介质的表面时,可以将表面活性物质的溶液添加到元素化合物的水溶液中,从而提高粘附强度。
添加元素化合物后,将多孔介质在30-250℃下干燥0.5-2小时。为了形成含油沸石、氧化铝、氧化硅、氧化钛、氧化锆、铝硅酸盐、硅酸铁、氧化铁、粘土或它们的任何组合的载体层,其总质量分数不小于5%总催化剂质量,每次浸渍后干燥和/或煅烧一次或多次。
接着,对具有元素化合物的多孔载体进行煅烧,以将所添加的元素化合物转变为氧化物形式。具有元素化合物的载体在250℃和1200℃之间的温度下煅烧2-8小时以形成沸石、氧化铝、氧化硅、氧化钛、氧化锆、铝硅酸盐、硅酸铁、氧化铁的各种变体、粘土或它们以单独形式或彼此组合的任何组合的二次层。氧化铝二次层的特征是厚度为10μm至2000μm,比表面积至少为20m2/g,孔隙体积0.1至1.0cm3/g,孔径大于5nm,至少占总空隙体积的50%。催化剂总组合物中的二次氧化铝载体至少为5%(重量)。使用一层厚度不小于10微米且不大于2000微米且总量不小于5%的二次层氧化铝,是由于需要形成一定量的活性相来转化稠油、重油和超重渣油的烃类。
在第三阶段,将活性成分施加到具有第二载体层(二级载体)的多孔载体的表面上。选自镍、钴、钼、钨化合物或其任意组合的活性组分的引入在将辅助载体固定在高多孔载体上的阶段和/或通过用高多孔载体浸渍高多孔载体进行。固定辅助载体。在施加活性成分化合物后,催化剂在50℃至250℃的温度下干燥1-2小时,并在250℃至800℃的温度下煅烧2-8小时。
实施例1:
催化剂的制备方法是用醋酸锌和钼酸铵溶液依次浸渍含δ-Al2O3二级载体的高孔隙度镍载体。多孔镍载体的孔隙度为87%,平均孔径为1.2mm。δ-Al2O3和Fe2O3二级载体的比表面积为164m2/g,孔体积为0.58cm3/g,直径大于5nm的孔隙,占总孔体积的63%。δ-Al2O3层厚度为45μm。二级载体的特征是存在Bronsted和Lewis中强酸位,根据氨的升温脱附,氨气脱附峰温度范围为250-350℃和350℃以上,脱附量分别为174和79μmol/g,Bronsted-Lewis的酸比为2.2:1.0。
首先将含δ-Al2O3和Fe2O3(81.1g)二级载体的高孔隙度镍载体放入混合室,加入200ml含有25.05g醋酸锌的水溶液,在80℃温度下浸渍3小时。在用醋酸锌溶液浸渍后,在90℃的温度下放置2小时从而去除溶剂。然后,在60℃温度下干燥2小时,并在500℃温度下煅烧4小时具,以将锌转化为氧化物状态。
接下来,将载体放置在混合室中,加入450ml含有139.44g钼酸铵的水溶液。在80℃温度下在浸渍2小时。在用钼酸铵浸渍载体后,在110℃温度下放置3小时从而去除溶剂。然后,在250℃温度下干燥1小时,再在500℃温度下煅烧2小时,最后在150℃的氢气中还原2小时。
成品催化剂的特征是沿催化剂床横截面对角线的温度下降为0.7℃,Thiel(Ψ)模量为0.12。
催化剂成分如下(质量分数):
Zn–7.4%;
Mo–11.5%;
δ-Al2O3+Fe2O3–7.3%;
高孔隙度镍载体–73.8%。
该样品的催化试验结果如表3-4所示。
实施例2:
催化剂的制备方法是用硝酸铯、硝酸镍和硝酸钴溶液依次浸渍具有δ-Al2O3和TiO2二级载体的高孔隙度铁载体。高孔隙度铁载体的孔隙率为85%,平均孔径为0.5mm。二级载体δ-Al2O3和TiO2的比表面积为225m2/g,孔体积为0.1cm3/g,直径大于5nm的孔占总孔体积的50%。δ-Al2O3和TiO2层的厚度为10μm。二级载体的特征是存在Bronsted和Lewis中强酸位,根据氨的升温脱附,氨气脱附峰温度范围为250-350℃和350℃以上,脱附量分别为15和3μmol/g,Bronsted-Lewis的酸比为5.0:1.0。
将具有δ-Al2O3和TiO2(100g)二级载体的高孔隙度铁载体放入混合室中,加入300ml含有124g硝酸铈的水溶液。在60℃温度下浸渍3小时。用硝酸铈水溶液浸渍载体后,在90℃的温度下放置2小时以去除溶剂。然后,在110℃温度下干燥载体1小时,再在600℃温度下煅烧8小时,以将硝酸铈转化为氧化铈。
接下来,将载体放入混合室中,添加300ml含有49.32g硝酸镍和41.43g硝酸钴的水溶液。在70℃浸渍溶液温度下浸渍3小时。用硝酸镍和硝酸钴浸渍载体后,在150℃温度下放置2小时以去除溶剂。然后,将浸渍有硝酸镍和硝酸钴的载体在200℃温度下干燥2小时,接着在800℃温度下煅烧4小时,最后在200℃的氢气中还原2小时。
成品催化剂的特征是沿催化剂床横截面对角线的温度下降为0.5℃,Thiel模量(Ψ)为0.24。
催化剂成分如下(质量分数):
Ce–40.0%;
Ni–10.0%;
Co–8.4%;
δ-Al2O3+TiO2–9.8%;
高孔隙度铁载体–31.8%。
该样品的催化试验结果如表3-4所示。
实施例3:
催化剂的制备方法是用醋酸镁和硝酸镍溶液依次浸渍具有硅酸铝二级载体的高孔隙度多孔铝载体。铝载体孔隙率为94%,平均孔径为2.4mm。二级载体硅酸铝的比表面积为40m2/g,孔体积为0.83cm3/g,直径大于5nm的中孔,占总孔体积的87%。硅酸铝盐二级载体层的厚度为263μm。二级载体的特征是存在Bronsted和Lewis中强酸位,根据氨的升温脱附,氨气脱附峰温度范围为250-350℃和350℃以上,脱附量分别为1和1μmol/g,Bronsted-Lewis的酸比为1.0:1.0。
将具有硅酸铝二级载体的多孔铝载体(100g)放置在混合室中,添加100ml含有0.45g醋酸镁的水溶液。在70℃温度下浸渍3小时。在用醋酸镁水溶液浸渍载体后,在90℃的温度下放置1小时以去除溶剂。然后,在50℃温度下干燥载体2小时,并在250℃温度下煅烧5小时,以将起始醋酸镁转化为氧化镁。
接下来,将载体放置在混合室中,添加200ml含有84,84g硝酸镍的水溶液。在60℃温度下浸渍2小时。用硝酸镍浸渍载体后,在110℃温度下1小时以去除溶剂。然后在150℃的温度下干燥载体2小时,再在600℃的温度下煅烧8小时,最后在400℃的氢气中还原3小时。
成品催化剂的特征是沿催化剂床横截面对角线的温度下降为0.4℃,Thiel(Ψ)模量为0.07。
催化剂成分如下(质量分数):
Mg–0.05%;
Ni–40.0%;
Al2O3+SiO2–5.0%;
高孔隙度铝载体–54.95%。
该样品的催化试验结果如表3-4所示。
实施例4:
该催化剂制备方法是用硝酸铜、钼酸铵和钨酸溶液依次浸渍具有γ-Al2O3和ZrO2二级载体的高孔隙度多孔α-Al2O3载体。α-Al2O3多孔载体的孔隙度为90%,平均孔径为3.7mm。二级载体γ-Al2O3和ZrO2的比表面积为20m2/g,孔体积为1.0cm3/g,直径大于5nm的孔隙,占总孔体积的94%。二级载体的厚度为523μm。二级载体的特征是存在Bronsted和Lewis中强酸位,根据氨的升温脱附,氨气脱附峰温度范围为250-350℃和350℃以上,脱附量分别为1500和238μmol/g,Bronsted-Lewis的酸比为6.3:1.0。
将具有γ-Al2O3和ZrO2二级载体的高孔隙度多孔α-Al2O3载体(100g)放入混合室,加入300ml含有53.65g硝酸铜的水溶液。在60℃温度下浸渍3小时。在用硝酸铜水溶液浸渍载体后,在90℃温度下放置2小时以去除溶剂。然后,在250℃温度下干燥载体,再在800℃温度下煅烧5小时,以将硝酸铜转化为氧化铜。
接下来,将载体放置在混合室中,添加400ml含有145.5g钼酸铵和10.87g钨酸的水溶液。在50℃的温度下浸渍1小时。用钼酸铵和钨酸浸渍载体后,在120℃温度下放置2小时以去除溶剂。然后,将浸渍有钼酸铵和钨酸的载体在120℃温度下干燥6小时,再在600℃温度下煅烧3小时,最后在300℃的氢气中还原4小时。
成品催化剂的特征是沿催化剂床横截面对角线的温度下降为0.5℃,Thiel(Ψ)模量为0.07。
催化剂成分如下(质量分数):
Cu–11.6%;
Mo–12.0%;
W–8.0%;
γ-Al2O3+ZrO2–10.3%;
无机多孔载体α-Al2O3–58.1%。
该样品的催化试验结果如表3-4所示。
实施例5:
催化剂的制备方法是用硝酸钴溶液浸渍具有δ-Al2O3和ZSM-5沸石二级载体的高孔隙度α-Al2O3载体。α-Al2O3载体的孔隙度为91%,平均孔径为4.1mm。二级载体δ-Al2O3和ZSM-5沸石的比表面积为146m2/g,孔体积为0.58cm3/g,直径大于5nm的孔隙,共占总孔体积的73%。δ-Al2O3和ZSM-5沸石的厚度为2000μm。二级载体的特征是存在Bronsted和Lewis中强酸位,根据氨的升温脱附,氨气脱附峰温度范围为250-350℃和350℃以上,脱附量分别为300和1500μmol/g,Bronsted-Lewis的酸比为1.0:5.0。
将具有δ-Al2O3和ZSM-5沸石二级载体的α-Al2O3载体(100g)放置在混合室中,添加300ml含有0.25g硝酸钴的水溶液。在70℃温度下浸渍3小时。硝酸钴水溶液浸渍后,在90℃的温度下放置2小时以去除溶剂。然后,在50℃的温度下干燥2小时,再在500℃的温度下煅烧6小时,最后在400℃的氢气中还原4小时。
成品催化剂的特征是沿催化剂床横截面对角线的温差为0.3℃,Thiel(Ψ)模量为0.15。
催化剂成分如下(质量分数):
Co–0.05%;
δ-Al2O3+ZSM-5–12.6%;
无机多孔载体α-Al2O3–87.35%。
该样品的催化试验结果如表3-4所示。
实施例6:
催化剂的制备方法是用硝酸镍和硝酸钴水溶液浸渍具有SiO2和FeSiO3二级载体的高孔隙度α-Al2O3载体。α-Al2O3的孔隙度为94%,平均孔径为6.0mm。二级载体SiO2和FeSiO3的比表面积为85m2/g,孔体积为0.73cm3/g,直径大于5nm的孔,共同占总孔体积的85%。SiO2和FeSiO3的厚度为734μm。二级载体的特征是存在Bronsted和Lewis中强酸位,根据氨的升温脱附,氨气脱附峰温度范围为250-350℃和350℃以上,脱附量分别为35和3.5μmol/g,Bronsted-Lewis的酸比为10.0:1.0。
将具有SiO2和FeSiO3二级载体的高孔隙度α-Al2O3载体(100g)放置在混合室中,添加300ml含有25.15g硝酸镍和18.74g硝酸钴的水溶液。在60℃的温度下浸渍2小时。用硝酸镍和硝酸钴水溶液浸渍载体后,在90℃温度下放置3小时以去除溶剂。然后,在110℃的温度下干燥2小时,再在250℃的温度下煅烧6小时,最后在500℃的氢气中还原2小时。
成品催化剂的特征是沿催化剂床横截面对角线的温度下降为0.6℃,Thiel(Ψ)模量–0.13。
催化剂成分如下(质量分数):
Ni–5.1%;
Co–3.8%;
SiO2+FeSiO3–40.0%;
无机多孔载体α-Al2O3–51.1%。
该样品的催化试验结果如表3-4所示。
对比例1(即样品7)
铝硅酸盐在直径为150nm或更大的聚合聚苯乙烯纳米球载体上制备。使用四乙氧基硅烷、胶溶氢氧化铝的水溶液制备。
将载体原料造粒,将得到的颗粒风干一天,然后将模板在950℃空气中退火。所得载体材料具有规则的大空隙结构,平均直径为150nm。
将获得的载体浸渍有活性成分的溶液。浸渍溶液含有钴和钼化合物-
(NH4)6(Mo7O24)·4H2O和Co(NO3)2·6H2O。浸渍后的载体在室温下干燥24小时并在450℃空气中煅烧4小时。
得到的催化剂为直径2.5mm的圆柱形颗粒。总空隙体积为0.61cm3/g,比表面积为102m2/g。催化剂成分如下(质量分数):
Al2O3/SiO2–72%;
Co–8.7%;
Mo–19.3%。
对比例2(样品8)
通过在氢氧化铝粉末中加入蒸馏水、HNO3和载体,获得氧化铝Al2O3样品。载体是直径为150nm或更大的聚合聚苯乙烯纳米球。然后将糊状物制成直径为2.5毫米的颗粒。将粒料风干24小时并在950℃煅烧5小时。氧化铝样品具有规则的空隙结构,平均尺寸为146nm。将获得的载体浸渍有活性成分的溶液。浸渍溶液含有钴和钼化合物-
(NH4)6(Mo7O24)·4H2O和Co(NO3)2·6H2O。浸渍后的载体在室温下干燥24小时并在空气中在450℃下煅烧4小时。
得到的催化剂为直径为2.5mm的圆柱形颗粒。孔隙体积为0.55cm3/g,比表面积为112m2/g。该催化剂含有7.2%钴和19.5%钼。
催化剂的组成如下:
Co–7.2%;
Mo–19.5%;
Al2O3–73.3%。
对比例3(样品9)
通过在氢氧化铝粉末中加入蒸馏水、HNO3和载体,获得氧化铝Al2O3载体。载体是直径为100nm或更大的聚合聚苯乙烯纳米球。然后将糊状物制成直径为2.5毫米的颗粒。将粒料风干24小时并在950℃煅烧4小时。氧化铝样品具有规则的大孔空间结构,平均尺寸为100nm。将获得的载体浸渍有活性成分的溶液。浸渍溶液含有钴和钼化合物-
(NH4)6(Mo7O24)·4H2O和Co(NO3)2·6H2O。浸渍后的载体在室温下干燥24小时并在空气中在450℃下煅烧4小时。
得到的催化剂为直径为2.5mm的圆柱形颗粒。孔隙体积为0.49cm3/g,比表面积为134m2/g。该催化剂含有8.1%钴和17.8%钼。
催化剂的组成如下:
Co–8.1%;
Mo–17.8%;
Al2O3–74.1%。
根据标准Barrett-Joyner-Hyland程序,比表面积采用低温氮气吸附法(BET)测定。测定多孔催化剂参数的方法在ASTMD 3663-99《研究催化剂和催化剂载体的表面积和孔体积的标准方法》中有所描述。
载体和催化剂的相组成通过X射线衍射测定。X射线衍射图是在衍射光束上使用长波长CuK辐射和石墨单色器拍摄的。2θ角度记录范围为5到95度。
特超稠油催化加氢改质测试是在具有固定催化剂层的绝热反应器中进行的,温度为350-415℃,压力为40kgp/cm2,特超稠油的流速每小时14mL。根据氢气与原料的体积比为50-100nL/L,向反应器中额外供应氢气。实验前中使用的原料是运动粘度为3000cSt的稠油(表3)。使用Brookfield DV2T设备测量初始油和改质后油的粘度。
用液相吸附色谱法研究了初始油和改质后油的基团组成。原始油中含有49.65%油质组分(烷烃、环烷烃和单芳烃);40.12%胶质(苯胶质(聚芳烃)和酒精-苯(酸)胶质);10.23%沥青质(表3)。
通过X射线荧光分析初始油和改质油的元素组成。原始油含硫3.84%(表4)。
使用NETZSCH TG 209F1 Libra仪器在30-800℃的温度范围内在坩埚中以10K/min的加热速率对油样进行热重分析以确定馏分组成;在加热开始之前,所有样品在30℃下恒温放置5分钟。反应气体(氮气)的流量设定为30ml/min,保护气体(氮气)流量20mL/min。每种油的样品测量一次;样品的重量范围为4至7毫克。
使用AutoChem 2950HP分析仪进行氨热脱附试验,以确定Bronsted和Lewis酸位点的浓度。将0.5g的样品装入石英反应器中,然后在设备的电炉在550℃脱气,加热速率为10℃/min。载气(He)进料速率10ml/min。该载体在室温下用10%NH3在He中的混合物饱和一小时。然后在100℃下用氩气吹扫样品以去除物理吸附的氨。在25-700℃的温度范围内记录解吸光谱。测定误差为±10%。
在催化剂用于加氢改质反应的测试中评估了传热和传质指数。该方法的本质是测量沿位于催化剂层中心的反应器横截面轴线的最大温差。反应器的横截面直径为30mm。
根据计算值Ψ-Thiel模量估计扩散效率指标。Ψ<0.5表示过程发生在动力学区,表面利用程度接近统一,没有扩散限制。Ψ>2.5表示该过程在内部扩散区域进行,仅使用受表面层限制的部分催化剂,需考虑扩散限制。
表1-2给出了稠油加氢催化改质试验的催化剂初始数据,表3-4给出了试验结果。表1-4中的序号7为无载体催化剂的实验结果。在表4中,气相的含量反应了轻烃形成的量。
表1合成的加氢改质催化剂的基本参数
注:HPCM–无机多孔载体;ΔТ–催化剂层的温度梯度,℃;Ψ–Thiele模量;样品7组成(质量),%:Al2O3/SiO2–72;Co–8.7;Mo–19.3。
表2合成的加氢改质催化剂的基本参数
注:HPCM–无机多孔载体;ΔТ–催化剂层的温度梯度,℃;Ψ–Thiele模量;样品7组成(质量),%:Al2O3/SiO2–72;Co–8.7;Mo–19.3。
表3加氢改质过程中催化剂测试结果
表4加氢改质过程中催化剂测试结果
从上表可以看出,与催化剂(序号7)相比,本专利方法合成的催化剂在稠油加氢改质中的活性更高,催化剂成分的选择性也更广。这是因为使用了具有二级载体的无机多孔载体,使活性组分在催化剂表面上有最佳分布,反应分子具有大量活性位点,使质量和热传递的效率增加,消除了起始化合物和反应产物运输传递过程中的扩散限制,抑制焦炭生成,避免碳沉积物对孔隙的堵塞。这些特性有利于加快稠油中大分子化合物的处理速度,延长催化剂的使用周期,改质后稠油中的硫含量也大幅降低。
催化剂的二级载体存在Bronsted和Lewis中强酸位点,氨气脱附峰温度范围为250-350℃和350℃以上,脱附量分别为1-1500和1-1500μmol/g,Bronsted-Lewis酸比为1-10:1-5。这种特征可以确保粘性油、重质油和超重油分子加氢改质的速率高,油组分产率高,气相的碳氢化合物和焦炭的形成速率和产率低。
最后应当说明的是,以上内容仅用以说明本发明的技术方案,而非对本发明保护范围的限制,本领域的普通技术人员对本发明的技术方案进行的简单修改或者等同替换,均不脱离本发明技术方案的实质和范围。
Claims (10)
1.一种催化剂,其特征在于:包括无机多孔载体、二级载体和活性成分;所述二级载体的原料包括沸石、氧化铝、氧化铁、氧化硅、氧化钛、氧化锆、硅酸铝、硅酸铁和粘土中的一种或多种。
2.根据权利要求1所述的催化剂,其特征在于:所述无机多孔载体的起始金属包括镍、铬、铜、铁、钛、铝、氧化铝和氧化铁中的一种或多种。
3.根据权利要求1所述的催化剂,其特征在于:所述无机多孔载体的孔隙率在85%以上。
4.根据权利要求1所述的催化剂,其特征在于:所述二级载体固定在无机多孔载体上,所述活性成分固定在二级载体上。
5.根据权利要求1所述的催化剂,其特征在于:按重量百分比计,包括:5-40%二级载体和0.05-40%活性成分和余量无机多孔载体。
6.根据权利要求1所述的催化剂,其特征在于:所述活性成分包括:镍、钴、钼或钨的化合物中的一种或多种。
7.根据权利要求1所述的催化剂,其特征在于:所述催化剂还包括修饰元素。
8.根据权利要求7所述的催化剂,其特征在于:所述修饰元素包括K、Na、Mg、Zn、Cu、Re、Bi、Mn、Ba、Sn、B、Ce、Cs、Fe、Cr、Ti、Zr、Si和稀土元素中的一种或多种。
9.如权利要求1-6任一项所述的催化剂的制备方法,其特征在于:包括以下步骤:
S1:无机多孔载体的制备:将金属通过电化学沉积法或滑移法制得;
S2:向无机多孔载体中加入含有二级载体初始元素的溶液中,浸渍,干燥和/或煅烧,得到物料A;
S3:将物料A置于含有活性成分的水溶液中,加热浸渍,再次加热去除溶剂,干燥、煅烧、还原,即得催化剂。
10.如权利要求7或8所述的催化剂的制备方法,其特征在于:包括以下步骤:
(1)无机多孔载体的制备:将金属通过电化学沉积法或滑移法制得;
(2)向无机多孔载体中加入含有二级载体初始元素的溶液中,浸渍,干燥和/或煅烧,得到物料A;
(3)将物料A浸渍在含有修饰元素的化合物的水溶液中;加热去除溶剂,干燥,煅烧;得到物料B;
(4)将物料B置于含有活性成分的水溶液中,加热浸渍,再次加热去除溶剂,干燥、煅烧、还原,即得催化剂。
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