CN109692685B - 加氢精制催化剂的制备方法 - Google Patents
加氢精制催化剂的制备方法 Download PDFInfo
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- CN109692685B CN109692685B CN201710984490.7A CN201710984490A CN109692685B CN 109692685 B CN109692685 B CN 109692685B CN 201710984490 A CN201710984490 A CN 201710984490A CN 109692685 B CN109692685 B CN 109692685B
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- MOWMLACGTDMJRV-UHFFFAOYSA-N nickel tungsten Chemical compound [Ni].[W] MOWMLACGTDMJRV-UHFFFAOYSA-N 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 125000001477 organic nitrogen 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
- 239000003208 petroleum Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000005987 sulfurization reaction Methods 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
- 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
- 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
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
-
- B01J35/615—
-
- B01J35/633—
-
- B01J35/647—
-
- 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
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
- 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
-
- 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
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
Description
催化剂编号 | A | B | C | D | E | F | G | H |
NiO,wt% | 19 | 22 | 20 | 16 | 19 | 19 | 19 | 19 |
WO<sub>3</sub>,wt% | 35 | 28 | 32 | 33 | 35 | 35 | 35 | 35 |
MoO<sub>3</sub>,wt% | 18 | 18 | 15 | 20 | 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 | 197 | 205 | 199 | 196 | 175 | 179 | 219 | 225 |
孔容,mL/g | 0.301 | 0.308 | 0.305 | 0.297 | 0.271 | 0.273 | 0.325 | 0.334 |
机械强度,N/mm | 16.6 | 17.2 | 17.6 | 18.3 | 16.7 | 17.2 | 15.8 | 14.7 |
孔分布,% | ||||||||
<3nm | 12.23 | 12.58 | 13.06 | 13.42 | 65.16 | 63.81 | 11.51 | 20.18 |
3nm~10nm | 64.65 | 64.05 | 64.84 | 65.05 | 20.27 | 21.69 | 61.52 | 40.56 |
10nm~15nm | 10.56 | 10.91 | 10.44 | 10.28 | 8.03 | 9.12 | 23.47 | 30.24 |
>15nm | 12.56 | 12.46 | 11.66 | 11.25 | 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 | 8.38 | 5.05 |
B | 8.35 | 4.98 |
C | 8.28 | 5.02 |
D | 8.22 | 5.04 |
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 | 4.26 | 4.02 | 4.47 | 4.37 | 30.22 | 32.56 | 24.98 | 20.56 |
4.0至小于7.0层 | 11.32 | 10.14 | 10.86 | 12.05 | 66.22 | 64.98 | 71.26 | 74.26 |
7.0~9.0层 | 73.98 | 74.21 | 73.61 | 73.05 | 3.56 | 2.46 | 3.76 | 5.18 |
>9.0层 | 10.44 | 11.63 | 11.06 | 10.53 | - | - | - | - |
长度分布,% | ||||||||
<2.0nm | 5.08 | 6.21 | 6.14 | 5.18 | 1.19 | 1.23 | 1.09 | 1.54 |
2.0至小于4.0nm | 14.92 | 13.96 | 14.95 | 14.64 | 4.58 | 5.26 | 4.98 | 4.74 |
4.0~6.0nm | 73.62 | 73.15 | 72.19 | 73.36 | 8.27 | 8.56 | 8.69 | 8.19 |
大于6.0至8.0nm | 5.58 | 5.82 | 5.73 | 5.89 | 65.17 | 64.21 | 65.59 | 66.58 |
>8.0nm | 0.80 | 0.86 | 0.99 | 0.93 | 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> | 0.8705 | 0.8708 | 0.8697 | 0.8711 |
馏程范围,℃ | 170-371 | 168-372 | 174-372 | 170-372 |
S,µg/g | 9.2 | 8.1 | 8.7 | 8.5 |
N,µg/g | 9.1 | 8.5 | 8.8 | 8.4 |
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 | 9.2 | 8.1 | 8.7 | 8.5 | 265.6 |
C<sub>1</sub>-DBT,µg/g | 0 | 0 | 0 | 0 | 48.3 |
4- BMDBT,µg/g | 2.0 | 1.6 | 1.9 | 1.7 | 69.2 |
6-BMDBT,µg/g | 2.0 | 1.8 | 1.8 | 1.9 | 65.6 |
4,6- BMDBT,µg/g | 5.2 | 4.7 | 5.0 | 4.9 | 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 | 9.1 | 8.5 | 8.8 | 8.4 | 78.2 |
1- MCB,µg/g | 1.7 | 1.6 | 1.8 | 1.6 | 28.3 |
1,8-BMCB,µg/g | 2.0 | 2.0 | 2.0 | 1.8 | 34.9 |
1,4,8- TMCB,µg/g | 5.4 | 4.9 | 5.0 | 5.0 | 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 (28)
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