CN110038620B - 制备加氢裂化催化剂的方法 - Google Patents
制备加氢裂化催化剂的方法 Download PDFInfo
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- CN110038620B CN110038620B CN201810037419.2A CN201810037419A CN110038620B CN 110038620 B CN110038620 B CN 110038620B CN 201810037419 A CN201810037419 A CN 201810037419A CN 110038620 B CN110038620 B CN 110038620B
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- catalyst
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- aging
- hydrocracking catalyst
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- 239000003054 catalyst Substances 0.000 title claims abstract description 238
- 238000004517 catalytic hydrocracking Methods 0.000 title claims abstract description 115
- 238000004519 manufacturing process Methods 0.000 title description 2
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 62
- 239000011259 mixed solution Substances 0.000 claims abstract description 50
- 239000002808 molecular sieve Substances 0.000 claims abstract description 49
- 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 49
- 239000002002 slurry Substances 0.000 claims abstract description 46
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- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 22
- 150000007524 organic acids Chemical class 0.000 claims abstract description 21
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 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 16
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- 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
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- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- 239000004471 Glycine Substances 0.000 claims description 4
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- 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 4
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- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 claims description 4
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- 230000002431 foraging effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 230000007935 neutral effect Effects 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
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 125000001477 organic nitrogen group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- 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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
- C10G45/12—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
Abstract
Description
催化剂编号 | A | B | C | D | E | F | G | H |
催化剂组成 | ||||||||
NiO,wt% | 19 | 18 | 20 | 16 | 19 | 19 | 19 | 19 |
WO<sub>3</sub>,wt% | 28 | 30 | 32 | 34 | 28 | 28 | 28 | 28 |
SiO<sub>2</sub>,wt% | 22 | 23 | 21 | 23 | 22 | 22 | 22 | 22 |
Al<sub>2</sub>O<sub>3</sub>,wt% | 31 | 26 | 27 | 27 | 31 | 31 | 31 | 31 |
其它,wt% | - | ZrO<sub>2</sub>/3.0 | - | - | - | - | - | - |
催化剂性质 | ||||||||
比表面积,m<sup>2</sup>/g | 399 | 394 | 392 | 393 | 354 | 391 | 365 | 375 |
孔容,mL/g | 0.420 | 0.410 | 0.412 | 0.414 | 0.365 | 0.415 | 0.381 | 0.389 |
机械强度,N/mm | 19.4 | 19.5 | 19.6 | 19.9 | 17.7 | 17.8 | 17.1 | 17.3 |
孔分布,% | ||||||||
<4nm | 9.27 | 9.41 | 9.59 | 9.34 | 56.12 | 13.46 | 45.35 | 44.02 |
4nm~10nm | 67.35 | 67.12 | 67.23 | 67.17 | 30.12 | 46.08 | 38.05 | 38.39 |
10nm~15nm | 12.68 | 12.53 | 12.45 | 12.50 | 8.11 | 36.06 | 8.38 | 9.13 |
>15nm | 10.70 | 10.94 | 10.73 | 10.99 | 5.65 | 4.40 | 8.22 | 8.46 |
催化剂编号 | 平均堆积层数N<sub>A</sub> | 平均片层长度L<sub>A</sub>,nm |
A | 6.36 | 4.75 |
B | 6.29 | 4.79 |
C | 6.26 | 4.78 |
D | 6.28 | 4.80 |
E | 4.02 | 6.68 |
F | 4.18 | 6.89 |
G | 3.98 | 7.01 |
H | 4.05 | 6.92 |
催化剂编号 | A | B | C | D | E | F | G | H |
片层数分布,% | ||||||||
<3层 | 2.89 | 3.13 | 3.38 | 3.46 | 15.35 | 13.25 | 14.93 | 14.85 |
3至小于5层 | 10.11 | 10.57 | 10.44 | 10.68 | 76.25 | 75.95 | 75.09 | 75.26 |
5~7层 | 75.91 | 75.62 | 75.51 | 75.27 | 7.38 | 9.05 | 8.11 | 7.91 |
>7层 | 11.09 | 10.68 | 10.67 | 10.59 | 1.02 | 1.75 | 1.87 | 1.98 |
长度分布,% | ||||||||
<4nm | 17.16 | 17.37 | 17.40 | 17.39 | 5.69 | 5.26 | 6. 08 | 4.99 |
4~6nm | 76.54 | 76.03 | 75.83 | 76.07 | 12.36 | 13.95 | 14.02 | 14.21 |
大于6至8nm | 5.48 | 5.55 | 5.61 | 5.41 | 71.25 | 72.22 | 71.94 | 72.08 |
>8nm | 0.82 | 1.05 | 1.16 | 1.13 | 10.70 | 8.57 | 7.96 | 8.72 |
项目 | 分析结果 |
密度(20℃),g/cm<sup>3</sup> | 0.9205 |
馏程范围,℃ | 314-539 |
S,µg/g | 10100 |
N,µg/g | 1920 |
残炭,wt% | 0.18 |
凝点,℃ | 33 |
催化剂编号 | A | B | C | D |
反应温度,℃ | 389 | 390 | 389 | 390 |
进料中氮含量,µg/g | 92.6 | 100.5 | 79.6 | 91.9 |
产品分布和性质,wt% | ||||
重石脑油(82~138℃) | ||||
收率,wt% | 8.1 | 7.8 | 7.7 | 8.0 |
芳潜,wt% | 52.6 | 52.5 | 52.8 | 52.9 |
喷气燃料(138℃~249℃) | ||||
收率,wt% | 28.4 | 28.3 | 28.1 | 28.2 |
烟点,mm | 32 | 32 | 31 | 32 |
柴油(249℃~371℃) | ||||
收率,wt% | 28.5 | 28.4 | 28.5 | 28.5 |
十六烷值 | 70.9 | 70.2 | 70.6 | 70.1 |
尾油(>371℃) | ||||
收率,wt% | 30.4 | 30.5 | 30.6 | 30.5 |
BMCI值 | 6.2 | 6.6 | 6.3 | 6.8 |
中油选择性,wt% | 81.8 | 81.6 | 81.6 | 81.6 |
催化剂编号 | E | F | G | H |
反应温度,℃ | 396 | 396 | 395 | 396 |
进料中氮含量,µg/g | 90.6 | 105.9 | 102.7 | 89.4 |
产品分布,wt% | ||||
重石脑油(82~138℃) | ||||
收率,wt% | 9.8 | 10.0 | 9.9 | 9.7 |
芳潜,wt% | 63.6 | 62.1 | 63.3 | 62.8 |
喷气燃料(138℃~249℃) | ||||
收率,wt% | 18.2 | 18.8 | 19.0 | 18.9 |
烟点,mm | 22 | 24 | 24 | 23 |
柴油(249℃~371℃) | ||||
收率,wt% | 20.4 | 20.2 | 19.9 | 20.1 |
十六烷值 | 61.5 | 61.9 | 60.8 | 61.1 |
尾油(>371℃) | ||||
收率,wt% | 42.0 | 42.2 | 42.1 | 42.5 |
BMCI值 | 18.5 | 20.9 | 19.1 | 21.6 |
中油选择性,wt% | 66.5 | 67.5 | 67.1 | 67.8 |
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 (41)
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