CN111822038B - 一种加氢裂化催化剂的制备方法 - Google Patents
一种加氢裂化催化剂的制备方法 Download PDFInfo
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- CN111822038B CN111822038B CN201910297484.3A CN201910297484A CN111822038B CN 111822038 B CN111822038 B CN 111822038B CN 201910297484 A CN201910297484 A CN 201910297484A CN 111822038 B CN111822038 B CN 111822038B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 175
- 238000004517 catalytic hydrocracking Methods 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 89
- 230000032683 aging Effects 0.000 claims abstract description 76
- 238000006243 chemical reaction Methods 0.000 claims abstract description 73
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 62
- 150000003624 transition metals Chemical class 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 60
- 239000002002 slurry Substances 0.000 claims abstract description 44
- 239000002808 molecular sieve Substances 0.000 claims abstract description 34
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000011734 sodium Substances 0.000 claims abstract description 31
- 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 abstract description 30
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 29
- 239000001257 hydrogen Substances 0.000 claims abstract description 29
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- 238000001035 drying Methods 0.000 claims abstract description 17
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- 239000000243 solution Substances 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 30
- 239000002244 precipitate Substances 0.000 claims description 28
- 229910052759 nickel Inorganic materials 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 24
- 229910052721 tungsten Inorganic materials 0.000 claims description 24
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 22
- 239000010937 tungsten Substances 0.000 claims description 22
- -1 phosphine compound Chemical class 0.000 claims description 20
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 19
- 239000012752 auxiliary agent Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 15
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- 239000010703 silicon Substances 0.000 claims description 15
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 14
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 13
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- 235000019353 potassium silicate Nutrition 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 10
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- 238000009826 distribution Methods 0.000 claims description 9
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 8
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 claims description 8
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- 229940120146 EDTMP Drugs 0.000 claims description 6
- KIDJHPQACZGFTI-UHFFFAOYSA-N [6-[bis(phosphonomethyl)amino]hexyl-(phosphonomethyl)amino]methylphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCCCCCN(CP(O)(O)=O)CP(O)(O)=O KIDJHPQACZGFTI-UHFFFAOYSA-N 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 5
- 229940090960 diethylenetriamine pentamethylene phosphonic acid Drugs 0.000 claims description 5
- DUYCTCQXNHFCSJ-UHFFFAOYSA-N dtpmp Chemical compound OP(=O)(O)CN(CP(O)(O)=O)CCN(CP(O)(=O)O)CCN(CP(O)(O)=O)CP(O)(O)=O DUYCTCQXNHFCSJ-UHFFFAOYSA-N 0.000 claims description 5
- KDSNLYIMUZNERS-UHFFFAOYSA-N 2-methylpropanamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 claims description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
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- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims description 4
- DLNKOYKMWOXYQA-APPZFPTMSA-N phenylpropanolamine Chemical compound C[C@@H](N)[C@H](O)C1=CC=CC=C1 DLNKOYKMWOXYQA-APPZFPTMSA-N 0.000 claims description 4
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- BGQMOFGZRJUORO-UHFFFAOYSA-M tetrapropylammonium bromide Chemical compound [Br-].CCC[N+](CCC)(CCC)CCC BGQMOFGZRJUORO-UHFFFAOYSA-M 0.000 claims description 4
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- 239000000377 silicon dioxide Substances 0.000 claims description 3
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 2
- LMHAGAHDHRQIMB-UHFFFAOYSA-N 1,2-dichloro-1,2,3,3,4,4-hexafluorocyclobutane Chemical compound FC1(F)C(F)(F)C(F)(Cl)C1(F)Cl LMHAGAHDHRQIMB-UHFFFAOYSA-N 0.000 claims description 2
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 2
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims description 2
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- 239000012972 dimethylethanolamine Substances 0.000 claims description 2
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
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- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 2
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
- B01J29/16—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J29/166—Y-type faujasite
-
- B01J35/615—
-
- B01J35/633—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/20—Sulfiding
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G49/00—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00
- C10G49/02—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 characterised by the catalyst used
- C10G49/08—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
Abstract
Description
催化剂编号 | A | B | C | D | E | F |
催化剂组成 | ||||||
Ni<sub>2</sub>P,wt% | 35 | 35 | 34 | 32 | 35 | 35 |
WP,wt% | 15 | 19 | 18 | 21 | 15 | 15 |
SiO<sub>2</sub>,wt% | 24 | 21 | 23 | 22 | 24 | 24 |
Al<sub>2</sub>O<sub>3</sub>,wt% | 26 | 25 | 25 | 25 | 26 | 26 |
催化剂性质 | ||||||
比表面积,m<sup>2</sup>/g | 436 | 430 | 425 | 424 | 375 | 383 |
孔容,mL/g | 0.467 | 0.459 | 0.454 | 0.450 | 0.382 | 0.391 |
机械强度,N/mm | 19.3 | 20.6 | 20.8 | 21.0 | 17.9 | 18.6 |
孔分布,% | ||||||
<3nm | 5.56 | 6.26 | 6.26 | 6.45 | 48.58 | 40.09 |
3nm~10nm | 46.45 | 46.55 | 46.08 | 46.18 | 28.12 | 34.39 |
10nm~15nm | 37.51 | 36.32 | 36.72 | 36.61 | 15.11 | 17.28 |
>15nm | 10.48 | 10.87 | 10.94 | 10.76 | 8.19 | 8.24 |
过渡金属磷化物分散度,% | 27.68 | 26.54 | 26.90 | 26.83 | 10.89 | 13.13 |
过渡金属磷化物颗粒平均直径,nm | 5.5 | 5.7 | 5.9 | 5.7 | 18.2 | 19.5 |
项目 | 分析结果 |
密度(20℃),g/cm<sup>3</sup> | 0.9213 |
馏程范围,℃ | 328-541 |
S,µg/g | 12500 |
N,µg/g | 2120 |
残炭,wt% | 0.19 |
凝点,℃ | 34 |
催化剂编号 | A | B | C | D | E | F |
反应温度,℃ | 390 | 391 | 391 | 390 | 399 | 398 |
进料中氮含量,µg/g | 101.2 | 109.3 | 126.3 | 107.4 | 106.8 | 109.0 |
产品分布和性质 | ||||||
重石脑油(82~138℃) | ||||||
收率,wt% | 8.5 | 8.1 | 8.3 | 8.0 | 9.5 | 9.7 |
芳潜,wt% | 53.3 | 53.6 | 53.6 | 53.4 | 61.5 | 61.8 |
喷气燃料(138℃~249℃) | ||||||
收率,wt% | 28.3 | 28.2 | 28.1 | 28.1 | 18.0 | 18.4 |
烟点,mm | 34 | 33 | 33 | 32 | 23 | 24 |
柴油(249℃~371℃) | ||||||
收率,wt% | 28.6 | 28.7 | 28.6 | 28.8 | 20.5 | 20.1 |
十六烷值 | 71.5 | 71.2 | 71.6 | 71.0 | 61.0 | 60.7 |
尾油(>371℃) | ||||||
收率,wt% | 30.5 | 30.4 | 30.5 | 30.3 | 42.2 | 42.4 |
BMCI值 | 6.3 | 6.6 | 6.9 | 6.5 | 18.9 | 21.3 |
中油选择性,wt% | 81.9 | 81.7 | 81.6 | 81.6 | 66.7 | 66.8 |
相对结晶度,% | 95 |
晶胞参数,nm | 2.439 |
SiO<sub>2</sub>/Al<sub>2</sub>O<sub>3</sub>,mol/mol | 12.05 |
比表面积,m<sup>2</sup>/g | 839 |
孔容,mL/g | 0.506 |
1.7~10nm二次孔占总孔容,% | 48.0 |
红外总酸,mmol/g | 0.999 |
Na<sub>2</sub>O,wt% | 0.093 |
Claims (38)
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CN104588085A (zh) * | 2013-11-03 | 2015-05-06 | 中国石油化工股份有限公司 | 制备加氢裂化催化剂的方法 |
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