CN109692692A - 一种加氢精制催化剂的制备方法 - Google Patents
一种加氢精制催化剂的制备方法 Download PDFInfo
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- CN109692692A CN109692692A CN201710984467.8A CN201710984467A CN109692692A CN 109692692 A CN109692692 A CN 109692692A CN 201710984467 A CN201710984467 A CN 201710984467A CN 109692692 A CN109692692 A CN 109692692A
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- 239000011259 mixed solution Substances 0.000 claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- 239000002002 slurry Substances 0.000 claims abstract description 46
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- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 37
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- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 1
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- 240000000203 Salix gracilistyla Species 0.000 description 1
- 244000275012 Sesbania cannabina Species 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 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 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- WCOATMADISNSBV-UHFFFAOYSA-K diacetyloxyalumanyl acetate Chemical compound [Al+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WCOATMADISNSBV-UHFFFAOYSA-K 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000007327 hydrogenolysis reaction Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910000476 molybdenum oxide 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
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 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
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- 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
- B01J35/63—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
-
- 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
- B01J37/0215—Coating
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
-
- 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
- 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
- C10G45/06—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 nickel or cobalt metal, or compounds thereof
- C10G45/08—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 nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
Description
催化剂编号 | A | B | C | D | E | F | G | H |
Ni,以NiO计,wt% | 19 | 20 | 22 | 17 | 19 | 19 | 19 | 19 |
W,以WO<sub>3</sub>计,wt% | 35 | 28 | 25 | 34 | 35 | 35 | 35 | 35 |
Mo,以MoO<sub>3</sub>计,wt% | 18 | 17 | 18 | 15 | 18 | 18 | 18 | 18 |
有机助剂P1,wt% | 5 | 5 | 6 | 7 | - | - | - | - |
有机助剂P2,wt% | 3 | 4 | 4 | 4 | - | - | - | - |
Al,以Al<sub>2</sub>O<sub>3</sub>计,wt% | 余量 | 余量 | 余量 | 余量 | 余量 | 余量 | 余量 | 余量 |
其它/wt% | - | ZrO<sub>2</sub>/3.0 | - | - | - | - | - | - |
比表面积,m<sup>2</sup>/g | 206 | 201 | 199 | 198 | 175 | 179 | 219 | 225 |
孔容,mL/g | 0.318 | 0.312 | 0.310 | 0.311 | 0.271 | 0.273 | 0.325 | 0.334 |
机械强度,N/mm | 16.6 | 17.1 | 17.8 | 17.6 | 16.7 | 17.2 | 15.8 | 14.7 |
催化剂编号 | 平均堆叠层数N<sub>A</sub> | 平均长度L<sub>A</sub>,nm |
A | 8.42 | 4.92 |
B | 8.34 | 4.96 |
C | 8.29 | 4.94 |
D | 8.32 | 4.97 |
E | 4.88 | 7.92 |
F | 5.03 | 8.01 |
G | 5.97 | 7.85 |
H | 5.93 | 7.62 |
催化剂编号 | A | B | C | D | E | F | G | H |
片层数分布,% | ||||||||
<4.0层 | 3.18 | 3.21 | 3.33 | 3.26 | 30.22 | 32.56 | 24.98 | 20.56 |
4.0至小于7.0层 | 8.26 | 8.52 | 8.28 | 8.34 | 66.22 | 64.98 | 71.26 | 74.26 |
7.0~9.0层 | 75.02 | 75.31 | 75.49 | 75.56 | 3.56 | 2.46 | 3.76 | 5.18 |
>9.0层 | 13.54 | 12.96 | 12.90 | 12.84 | - | - | - | - |
长度分布,% | ||||||||
<2.0nm | 6.45 | 6.25 | 6.23 | 6.74 | 1.19 | 1.23 | 1.09 | 1.54 |
2.0至小于4.0nm | 13.56 | 13.41 | 13.32 | 13.37 | 4.58 | 5.26 | 4.98 | 4.74 |
4.0~6.0nm | 74.75 | 74.84 | 74.90 | 74.83 | 8.27 | 8.56 | 8.69 | 8.19 |
大于6.0至8.0nm | 4.35 | 4.31 | 4.62 | 4.15 | 65.17 | 64.21 | 65.59 | 66.58 |
>8.0nm | 0.89 | 1.19 | 0.93 | 0.91 | 20.79 | 20.74 | 19.65 | 18.95 |
项目 | 分析结果 |
密度(20℃),g/cm<sup>3</sup> | 0.9025 |
馏程范围,℃ | 162-375 |
S,µg/g | 5026 |
N,µg/g | 1024 |
催化剂编号 | A | B | C | D |
生成油密度(20℃),g/cm<sup>3</sup> | 0.8701 | 0.8702 | 0.8699 | 0.8697 |
馏程范围,℃ | 172-371 | 165-371 | 173-371 | 172-371 |
S,µg/g | 7.9 | 8.1 | 8.3 | 8.5 |
N,µg/g | 8.0 | 8.2 | 8.6 | 8.3 |
催化剂编号 | E | F | G | H |
生成油密度(20℃),g/cm<sup>3</sup> | 0.8856 | 0.8883 | 0.8804 | 0.8812 |
馏程范围,℃ | 173-374 | 172-374 | 176-373 | 175-373 |
S,µg/g | 265.6 | 260.2 | 217.5 | 228.6 |
N,µg/g | 78.2 | 74.8 | 60.9 | 62.1 |
催化剂编号 | A | B | C | D | E |
加氢精制油中硫含量,µg/g | 7.9 | 8.1 | 8.3 | 8.5 | 265.6 |
C<sub>1</sub>-DBT,µg/g | 0 | 0 | 0 | 0 | 48.3 |
4- BMDBT,µg/g | 1.8 | 1.7 | 1.6 | 1.8 | 69.2 |
6-BMDBT,µg/g | 1.7 | 1.8 | 1.8 | 1.9 | 65.6 |
4,6- BMDBT,µg/g | 4.4 | 4.6 | 4.9 | 4.8 | 82.5 |
催化剂编号 | F | G | H |
加氢精制油中硫含量,µg/g | 260.2 | 217.5 | 228.6 |
C<sub>1</sub>-DBT,µg/g | 40.7 | 33.4 | 37.8 |
4- BMDBT,µg/g | 61.5 | 54.9 | 56.5 |
6-BMDBT,µg/g | 68.4 | 56.3 | 60.3 |
4,6- BMDBT,µg/g | 89.6 | 72.9 | 74.0 |
催化剂编号 | A | B | C | D | E |
加氢精制油中氮含量,µg/g | 8.0 | 8.2 | 8.6 | 8.4 | 78.2 |
1- MCB,µg/g | 1.8 | 1.8 | 1.9 | 1.9 | 28.3 |
1,8-BMCB,µg/g | 1.9 | 2.0 | 2.1 | 2.0 | 34.9 |
1,4,8- TMCB,µg/g | 4.3 | 4.4 | 4.6 | 4.5 | 15.0 |
催化剂编号 | F | G | H |
加氢精制油中氮含量,µg/g | 74.8 | 60.9 | 62.1 |
1-MCB,µg/g | 24.2 | 18.1 | 17.8 |
1,8-BMCB,µg/g | 35.3 | 28.3 | 29.5 |
1,4,8-TMCB,µg/g | 15.3 | 14.5 | 14.8 |
Claims (19)
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CN114433205B (zh) * | 2020-10-19 | 2023-09-01 | 中国石油化工股份有限公司 | 一种体相加氢裂化催化剂的制备方法 |
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