JP5677446B2 - 改善された熱水安定性を有するニ成分修飾モレキュラーシーブ - Google Patents
改善された熱水安定性を有するニ成分修飾モレキュラーシーブ Download PDFInfo
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- JP5677446B2 JP5677446B2 JP2012535574A JP2012535574A JP5677446B2 JP 5677446 B2 JP5677446 B2 JP 5677446B2 JP 2012535574 A JP2012535574 A JP 2012535574A JP 2012535574 A JP2012535574 A JP 2012535574A JP 5677446 B2 JP5677446 B2 JP 5677446B2
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- Prior art keywords
- molecular sieve
- modified molecular
- aqueous solution
- hydrothermal stability
- phosphorus
- 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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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical class [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims description 146
- 239000002808 molecular sieve Substances 0.000 claims description 97
- 238000006243 chemical reaction Methods 0.000 claims description 61
- 239000000243 solution Substances 0.000 claims description 37
- 239000007864 aqueous solution Substances 0.000 claims description 33
- 229910052698 phosphorus Inorganic materials 0.000 claims description 30
- 239000011574 phosphorus Substances 0.000 claims description 30
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 29
- 229910052709 silver Inorganic materials 0.000 claims description 24
- 239000004332 silver Substances 0.000 claims description 24
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 22
- 238000004519 manufacturing process Methods 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- -1 silver ions Chemical class 0.000 claims description 7
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 6
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 239000004254 Ammonium phosphate Substances 0.000 claims description 3
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 3
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical compound [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 description 64
- 239000000203 mixture Substances 0.000 description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 51
- 239000012153 distilled water Substances 0.000 description 49
- 230000000694 effects Effects 0.000 description 41
- 230000032683 aging Effects 0.000 description 18
- 239000005995 Aluminium silicate Substances 0.000 description 17
- 235000012211 aluminium silicate Nutrition 0.000 description 17
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 17
- 101710134784 Agnoprotein Proteins 0.000 description 15
- 238000003756 stirring Methods 0.000 description 15
- 239000000725 suspension Substances 0.000 description 13
- 150000001336 alkenes Chemical class 0.000 description 11
- 230000004048 modification Effects 0.000 description 10
- 238000012986 modification Methods 0.000 description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 9
- 239000010457 zeolite Substances 0.000 description 9
- 229910021536 Zeolite Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 6
- 239000005977 Ethylene Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 238000002715 modification method Methods 0.000 description 6
- 229910052723 transition metal Inorganic materials 0.000 description 6
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 5
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 5
- 238000004523 catalytic cracking Methods 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- JRLPEMVDPFPYPJ-UHFFFAOYSA-N 1-ethyl-4-methylbenzene Chemical compound CCC1=CC=C(C)C=C1 JRLPEMVDPFPYPJ-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000006317 isomerization reaction Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 238000007348 radical reaction Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000004846 x-ray emission Methods 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 1
- 230000002152 alkylating effect Effects 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007233 catalytic pyrolysis Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002468 redox effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002352 steam pyrolysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
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- B01J37/0201—Impregnation
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C4/00—Preparation of hydrocarbons from hydrocarbons containing a larger number of carbon atoms
- C07C4/02—Preparation of hydrocarbons from hydrocarbons containing a larger number of carbon atoms by cracking a single hydrocarbon or a mixture of individually defined hydrocarbons or a normally gaseous hydrocarbon fraction
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- 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
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G11/14—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid catalysts
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Description
本発明の目的は、現状のモレキュラ―シーブ材料及び技術に関して、実質的に改善された熱水安定性を有する二成分修飾モレキュラ―シーブ及びその製造方法を提供することにある。
それぞれの実施例及び比較例における分析方法は以下の通りである。
18.6gの(NH4)2HPO4を400gの蒸留水に溶解する。100gのZSM-5モレキュラーシーブを溶液へ攪拌下加えて、pH値を3へ調整する。混合物を攪拌し、90℃の反応温度で120分間反応させて、次いで、濾過し、乾燥させて、その後、550℃で4時間焼成する。こうして得られたモレキュラ―シーブサンプルをPZD−1と標識する。
18.6gの(NH4)2HPO4を400gの蒸留水に溶解する。100gのZSM-5モレキュラーシーブを溶液へ攪拌下加えて、pH値を3へ調整する。混合物を攪拌し、20℃の反応温度で0.4MPaの反応圧力下、120分間反応させて、次いで、濾過し、乾燥させて、その後、550℃で4時間焼成する。こうして得られたモレキュラ―シーブサンプルをPZD−2と標識する。
18.6gの(NH4)2HPO4及び100gのZSM−5モレキュラーシーブを均質になるまで機械的に混合し、その後550℃で4時間焼成する。こうして得られたモレキュラ―シーブサンプルをPZD−3と標識する。
9.3gの(NH4)2HPO4を110gの蒸留水に溶解する。100gのZSM−5モレキュラーシーブを溶液に加え、300分間含浸させて、次いで、乾燥させて、その後500℃で4時間焼成する。こうして得られたモレキュラ―シーブサンプルをPZD−4と標識する。
18.6gのNH4H2PO4を400gの蒸留水に溶解する。100gのβモレキュラーシーブを溶液に攪拌下加え、pH値を2へ調整する。混合物を攪拌し、50℃の反応温度で60分間反応させて、次いで、濾過し、乾燥させて、その後600℃で2時間焼成する。こうして得られたモレキュラ―シーブサンプルをPβD−1と標識する。
18.6gの(NH4)2HPO4を400gの蒸留水に溶解する。100gのZSM−5モレキュラーシーブサンプルを溶液に攪拌下加え、その後、1.46gのAgNO3を含有する10mL溶液を加え、pH値を3へ調整する。混合物を攪拌し、120℃の反応温度で0.4MPaの反応圧力下120分間反応させて、次いで、濾過し、乾燥させて、その後550℃で4時間焼成する。こうして得られたモレキュラ―シーブサンプルをAPZD−5と標識する。
本発明は、本発明による修飾方法によって得られた最適な修飾モレキュラーシーブを提供する。前記モレキュラ―シーブは、無水ベースに基づき、アルミナに対するシリカ割合が15〜60の、88〜99wt%のモレキュラーシーブと、酸化物に基づき0.5〜10wt%のリンと、酸化物に基づき0.01〜2wt%の銀と、を含む。
Claims (14)
- 改善された熱水安定性を有する二成分修飾モレキュラーシーブを製造する方法であって、前記方法によれば、モレキュラーシーブをリン含有水溶液に加えて、pH1〜10で、70〜200℃の反応温度で、0.2〜1.2MPaの反応圧力の下で、10〜200分間反応させて、次いで、濾過し、乾燥させて、焼成し、リン修飾モレキュラーシーブを得て、前記リン修飾モレキュラーシーブを銀イオン含有水溶液に加えて、暗所で0〜100℃の反応温度で、30〜150分間反応させて、次いで、濾過し、乾燥させて、焼成し、二成分修飾モレキュラーシーブを製造することを特徴とする二成分修飾モレキュラーシーブを製造する方法。
- 前記モレキュラーシーブが、ZSM型、β型、Y型、又はMCM型モレキュラーシーブの内の1つであることを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記モレキュラーシーブが、アルミナに対するシリカの割合が15〜100の範囲である、ZSM型又はβ型モレキュラーシーブであることを特徴とする、請求項2記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記アルミナに対するシリカの割合が、15〜60の範囲であることを特徴とする、請求項3記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記リン含有水溶液が、リン酸の溶液、亜リン酸の溶液、可溶性リン酸塩の水溶液、及び/又は可溶性亜リン酸塩の水溶液であることを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記可溶性リン酸塩が、リン酸トリアンモニウム、リン酸水素二アンモニウム、無水リン酸アンモニウムの内の1つ又はそれ以上であることを特徴とする、請求項6記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記銀イオン含有水溶液が、硝酸銀の水溶液、酢酸銀の水溶液、又は両方であることを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記モレキュラーシーブを前記リン含有水溶液に加える時、pHを2〜7に調整することを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記モレキュラーシーブを前記リン含有水溶液に加える時、反応温度を90〜160℃に維持することを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記モレキュラーシーブを前記リン含有水溶液に加える時、反応圧力を0.2〜0.8MPa下に維持することを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記リン含有水溶液が、0.05〜1.0mol/Lの濃度を有することを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記銀イオン含有水溶液の前記モレキュラーシーブに対する重量比が、3:1〜7:1の範囲であることを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 前記銀イオン含有水溶液が、0.01〜0.1mol/Lの濃度を有することを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法。
- 二成分修飾モレキュラーシーブが、無水ベースに基づき、アルミナに対するシリカ割合が15〜60の、88〜99wt%のモレキュラーシーブと、酸化物に基づき0.5〜10wt%のリンと、酸化物に基づき0.01〜2wt%の銀と、を含むことを特徴とする、請求項1記載の改善された熱水安定性を有する二成分修飾モレキュラーシーブの製造方法によって製造された二成分修飾モレキュラーシーブ。
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CN110116021A (zh) * | 2018-02-07 | 2019-08-13 | 中国石油天然气股份有限公司 | 一种fcc催化剂中分子筛的双组元改性方法及其改性分子筛 |
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