CN110038618A - 加氢裂化催化剂的制备方法 - Google Patents
加氢裂化催化剂的制备方法 Download PDFInfo
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- CN110038618A CN110038618A CN201810037408.4A CN201810037408A CN110038618A CN 110038618 A CN110038618 A CN 110038618A CN 201810037408 A CN201810037408 A CN 201810037408A CN 110038618 A CN110038618 A CN 110038618A
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- Prior art keywords
- catalyst
- aging
- acid
- mixed solution
- hydrocracking catalyst
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- 239000003054 catalyst Substances 0.000 title claims abstract description 204
- 238000004517 catalytic hydrocracking Methods 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 230000032683 aging Effects 0.000 claims abstract description 90
- 239000011259 mixed solution Substances 0.000 claims abstract description 48
- 239000002002 slurry Substances 0.000 claims abstract description 45
- 239000002808 molecular sieve Substances 0.000 claims abstract description 40
- 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 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 33
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 31
- 239000004033 plastic Substances 0.000 claims abstract description 27
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 27
- 229920003023 plastic Polymers 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 19
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 16
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 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 10
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- 238000009826 distribution Methods 0.000 claims description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
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- VPTUPAVOBUEXMZ-UHFFFAOYSA-N (1-hydroxy-2-phosphonoethyl)phosphonic acid Chemical compound OP(=O)(O)C(O)CP(O)(O)=O VPTUPAVOBUEXMZ-UHFFFAOYSA-N 0.000 claims description 5
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- 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 4
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- 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 3
- DCEMCPAKSGRHCN-UHFFFAOYSA-N oxirane-2,3-dicarboxylic acid Chemical compound OC(=O)C1OC1C(O)=O DCEMCPAKSGRHCN-UHFFFAOYSA-N 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- IQEKRNXJPCBUAT-UHFFFAOYSA-N 2-[hydroperoxy(hydroxy)phosphoryl]acetic acid Chemical compound OOP(O)(=O)CC(O)=O IQEKRNXJPCBUAT-UHFFFAOYSA-N 0.000 claims description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
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- CFPOJWPDQWJEMO-UHFFFAOYSA-N 2-(1,2-dicarboxyethoxy)butanedioic acid Chemical compound OC(=O)CC(C(O)=O)OC(C(O)=O)CC(O)=O CFPOJWPDQWJEMO-UHFFFAOYSA-N 0.000 claims 1
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- 239000012752 auxiliary agent Substances 0.000 claims 1
- 238000003475 lamination Methods 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 125000003367 polycyclic group Chemical group 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 26
- 238000000465 moulding Methods 0.000 abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 37
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- 238000005984 hydrogenation reaction Methods 0.000 description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 24
- 229910052757 nitrogen Inorganic materials 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 15
- 229910021641 deionized water Inorganic materials 0.000 description 15
- 239000013049 sediment Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 230000002378 acidificating effect Effects 0.000 description 12
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 10
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- 150000002739 metals Chemical class 0.000 description 10
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 10
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- 230000008859 change Effects 0.000 description 7
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- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 7
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 4
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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 description 3
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- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
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- 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
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 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
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 238000006557 surface reaction Methods 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
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/617—500-1000 m2/g
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/633—Pore volume less than 0.5 ml/g
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/635—0.5-1.0 ml/g
-
- 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
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G11/02—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils characterised by the catalyst used
- C10G11/06—Sulfides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Catalysts (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
Description
催化剂编号 | A | B | C | D | E | F | G | H |
催化剂组成 | ||||||||
NiO,wt% | 19 | 18 | 16 | 22 | 19 | 19 | 19 | 19 |
WO<sub>3</sub>,wt% | 28 | 32 | 34 | 30 | 28 | 28 | 28 | 28 |
SiO<sub>2</sub>,wt% | 22 | 22 | 23 | 20 | 22 | 22 | 22 | 22 |
Al<sub>2</sub>O<sub>3</sub>,wt% | 31 | 26 | 27 | 28 | 31 | 31 | 31 | 31 |
其它,wt% | - | ZrO<sub>2</sub>/2.0 | - | - | - | - | - | - |
催化剂性质 | ||||||||
比表面积,m<sup>2</sup>/g | 380 | 385 | 382 | 379 | 354 | 391 | 365 | 375 |
孔容,mL/g | 0.397 | 0.405 | 0.399 | 0.395 | 0.365 | 0.415 | 0.381 | 0.389 |
机械强度,N/mm | 18.9 | 18.7 | 18.3 | 18.8 | 17.7 | 17.8 | 17.1 | 17.3 |
孔分布,% | ||||||||
<4nm | 14.12 | 12.94 | 12.86 | 13.42 | 56.12 | 13.46 | 45.35 | 44.02 |
4nm~10nm | 64.95 | 65.93 | 65.85 | 65.03 | 30.12 | 46.08 | 38.05 | 38.39 |
10nm~15nm | 10.69 | 10.61 | 10.49 | 10.20 | 8.11 | 36.06 | 8.38 | 9.13 |
>15nm | 10.24 | 10.52 | 10.80 | 11.35 | 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 | 6.13 | 4.91 |
B | 6.05 | 4.82 |
C | 6.08 | 4.88 |
D | 6.14 | 4.90 |
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 | 3.15 | 3.56 | 3.21 | 3.39 | 15.35 | 13.25 | 14.93 | 14.85 |
3至小于5层 | 10.49 | 12.21 | 12.66 | 11.61 | 76.25 | 75.95 | 75.09 | 75.26 |
5~7层 | 73.97 | 73.99 | 73.47 | 73.91 | 7.38 | 9.05 | 8.11 | 7.91 |
>7层 | 12.39 | 10.24 | 10.66 | 11.09 | 1.02 | 1.75 | 1.87 | 1.98 |
长度分布,% | ||||||||
<4nm | 18.06 | 18.15 | 17.96 | 17.59 | 5.69 | 5.26 | 6.08 | 4.99 |
4~6nm | 73.86 | 73.92 | 74.16 | 74.58 | 12.36 | 13.95 | 14.02 | 14.21 |
大于6至8nm | 6.88 | 6.69 | 6.15 | 6.23 | 71.25 | 72.22 | 71.94 | 72.08 |
>8nm | 1.20 | 1.24 | 1.73 | 1.60 | 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,℃ | 390 | 390 | 391 | 390 |
进料中氮含量,µg/g | 102.2 | 89.4 | 101.1 | 96.3 |
产品分布和性质,wt% | ||||
重石脑油(82~138℃) | ||||
收率,wt% | 7.8 | 8.2 | 7.9 | 8.0 |
芳潜,wt% | 53.1 | 53.2 | 52.3 | 52.7 |
喷气燃料(138℃~249℃) | ||||
收率,wt% | 27.9 | 27.8 | 28.0 | 28.8 |
烟点,mm | 31 | 32 | 31 | 31 |
柴油(249℃~371℃) | ||||
收率,wt% | 28.4 | 28.6 | 28.5 | 27.9 |
十六烷值 | 69.9 | 70.6 | 70.8 | 70.3 |
尾油(>371℃) | ||||
收率,wt% | 30.8 | 30.5 | 30.6 | 30.5 |
BMCI值 | 6.1 | 6.8 | 6.3 | 6.7 |
中油选择性,wt% | 81.3 | 81.1 | 81.4 | 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 (23)
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