CN110038585A - 一种加氢精制催化剂的制法 - Google Patents
一种加氢精制催化剂的制法 Download PDFInfo
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- CN110038585A CN110038585A CN201810037436.6A CN201810037436A CN110038585A CN 110038585 A CN110038585 A CN 110038585A CN 201810037436 A CN201810037436 A CN 201810037436A CN 110038585 A CN110038585 A CN 110038585A
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- aging
- catalyst
- mixed solution
- added
- hydrobon catalyst
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 239000002002 slurry Substances 0.000 claims abstract description 44
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000004033 plastic Substances 0.000 claims abstract description 36
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- 150000001412 amines Chemical class 0.000 claims abstract description 19
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- 239000002283 diesel fuel Substances 0.000 claims abstract description 11
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- 229940043237 diethanolamine Drugs 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
- 239000004744 fabric Substances 0.000 description 1
- 239000003292 glue Substances 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
- 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
- 230000000116 mitigating effect Effects 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 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
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 125000001741 organic sulfur group Chemical group 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
- 239000002245 particle Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 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
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
- B01J23/8885—Tungsten containing also 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
- 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
-
- 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
- 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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
-
- 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
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/04—Diesel oil
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Dispersion 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 |
NiO,wt% | 19 | 18 | 16 | 14 | 19 | 19 | 19 | 19 |
WO<sub>3</sub>,wt% | 35 | 34 | 36 | 38 | 35 | 35 | 35 | 35 |
MoO<sub>3</sub>,wt% | 18 | 16 | 17 | 18 | 18 | 18 | 18 | 18 |
Al<sub>2</sub>O<sub>3</sub>,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 | 207 | 197 | 201 | 202 | 175 | 179 | 219 | 225 |
孔容,mL/g | 0.306 | 0.295 | 0.301 | 0.299 | 0.271 | 0.273 | 0.325 | 0.334 |
机械强度,N/mm | 18.5 | 18.4 | 18.8 | 19.1 | 16.7 | 17.2 | 15.8 | 14.7 |
孔分布,% | ||||||||
<3nm | 9.31 | 9.64 | 9.59 | 9.44 | 65.16 | 63.81 | 11.51 | 20.18 |
3nm~10nm | 66.84 | 66.66 | 66.45 | 66.51 | 20.27 | 21.69 | 61.52 | 40.56 |
10nm~15nm | 11.43 | 11.35 | 11.68 | 11.59 | 8.03 | 9.12 | 23.47 | 30.24 |
>15nm | 12.42 | 12.35 | 12.28 | 12.46 | 6.54 | 5.38 | 3.50 | 9.02 |
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 | 8.40 | 4.90 |
B | 8.31 | 4.93 |
C | 8.33 | 4.92 |
D | 8.30 | 4.94 |
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 | 3.98 | 4.12 | 3.87 | 3.78 | 30.22 | 32.56 | 24.98 | 20.56 |
4.0至小于7.0层 | 10.29 | 10.45 | 10.56 | 11.01 | 66.22 | 64.98 | 71.26 | 74.26 |
7.0~9.0层 | 74.94 | 74.86 | 74.81 | 74.79 | 3.56 | 2.46 | 3.76 | 5.18 |
>9.0层 | 10.79 | 10.57 | 10.76 | 10.42 | - | - | - | - |
长度分布,% | ||||||||
<2.0nm | 5.82 | 5.78 | 5.84 | 5.79 | 1.19 | 1.23 | 1.09 | 1.54 |
2.0至小于4.0nm | 14.02 | 13.92 | 13.87 | 13.96 | 4.58 | 5.26 | 4.98 | 4.74 |
4.0~6.0nm | 74.01 | 73.52 | 73.43 | 73.39 | 8.27 | 8.56 | 8.69 | 8.19 |
大于6.0至8.0nm | 5.43 | 5.91 | 5.92 | 5.84 | 65.17 | 64.21 | 65.59 | 66.58 |
>8.0nm | 0.72 | 0.87 | 0.94 | 1.02 | 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> | 0.8695 | 0.8698 | 0.8699 | 0.8697 |
馏程范围,℃ | 172-371 | 171-371 | 170-371 | 174-371 |
S,µg/g | 7.3 | 7.7 | 7.9 | 7.6 |
N,µg/g | 7.7 | 8.0 | 8.0 | 7.9 |
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 | 7.3 | 7.7 | 7.9 | 7.6 | 265.6 |
C<sub>1</sub>-DBT,µg/g | 0 | 0 | 0 | 0 | 48.3 |
4- BMDBT,µg/g | 1.5 | 1.6 | 1.6 | 1.6 | 69.2 |
6-BMDBT,µg/g | 1.7 | 1.8 | 1.9 | 1.8 | 65.6 |
4,6- BMDBT,µg/g | 4.1 | 4.3 | 4.4 | 4.2 | 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 | 7.7 | 8.0 | 8.0 | 7.9 | 78.2 |
1- MCB,µg/g | 1.4 | 1.5 | 1.5 | 1.5 | 28.3 |
1,8-BMCB,µg/g | 1.8 | 1.8 | 1.9 | 1.8 | 34.9 |
1,4,8- TMCB,µg/g | 4.5 | 4.7 | 4.6 | 4.6 | 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 (20)
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