CN106552635A - The preparation method of high hydrothermal stability hydrogenation deoxidation catalyst - Google Patents
The preparation method of high hydrothermal stability hydrogenation deoxidation catalyst Download PDFInfo
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- CN106552635A CN106552635A CN201611012129.XA CN201611012129A CN106552635A CN 106552635 A CN106552635 A CN 106552635A CN 201611012129 A CN201611012129 A CN 201611012129A CN 106552635 A CN106552635 A CN 106552635A
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- preparation
- hydrogenation deoxidation
- deoxidation catalyst
- drying
- hydrothermal stability
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- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 22
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011777 magnesium Substances 0.000 claims abstract description 18
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 18
- -1 magnesium aluminate Chemical class 0.000 claims abstract description 18
- 239000011029 spinel Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 17
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000007493 shaping process Methods 0.000 claims abstract description 9
- 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 abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 4
- 229910026161 MgAl2O4 Inorganic materials 0.000 claims abstract description 4
- 239000004480 active ingredient Substances 0.000 claims abstract description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 239000000428 dust Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 244000275012 Sesbania cannabina Species 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 3
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 229920001971 elastomer Polymers 0.000 abstract 1
- 239000000806 elastomer Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 4
- 239000008158 vegetable oil Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 241000219782 Sesbania Species 0.000 description 2
- 239000003225 biodiesel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 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
- B01J23/88—Molybdenum
- B01J23/883—Molybdenum and nickel
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/12—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation
- C11C3/123—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation using catalysts based principally on nickel or derivates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method of high hydrothermal stability hydrogenation deoxidation catalyst, height is comprised the steps of：（1）The preparation of magnesium aluminate spinel：Magnesium aluminate spinel is prepared into as raw material with magnesium nitrate, aluminum nitrate and cetyl trimethylammonium bromide；（2）Prepare shaping carrier：Magnesium aluminate spinel, aluminum hydroxide solid elastomer and sesbania powder are mixed, and adds dust technology, Jing extruded mouldings, drying, cutting, roasting obtain shaping carrier MgAl2O4；（3）Carrying active ingredients prepare hydrogenation deoxidation catalyst：By shaping carrier, MoO and NiO, citric acid mix homogeneously, 12 h under room temperature, are stood, 110 DEG C of 3 h of drying in muffle furnace, 500 DEG C of 3 h of roasting are obtained hydrogenation deoxidation catalyst.The aperture of the carrier magnesium aluminate spinel that the method is prepared is larger, and the catalyst hydrogenation deoxy activity for preparing and hydrothermal stability are excellent.
Description
Technical field
The invention belongs to the preparation field of catalyst, and in particular to a kind of system of high hydrothermal stability hydrogenation deoxidation catalyst
Preparation Method.
Background technology
It is MgAl that magnesium aluminate spinel is chemical formula2O4Composite oxides, wherein, Mg2+Positioned at 1 tetrahedron space, Al3+
Positioned at the octahedral interstices of cubic structure.As magnesium aluminate spinel lattice tightness is big, hydrone is difficult to enter crystals, thus
With excellent hydrothermal stability, it is excellent novel catalyst carrier.Additionally, the resistance to chemical corrosion of magnesium aluminate spinel it is strong,
High mechanical strength.
With the increasingly increase of energy demand, petroleum resources more show scarcity.Vegetable oil is used as the reproducible green ring of one kind
Protect novel energy widely to be paid close attention to.Vegetable oil hydrogenation gained biodiesel with without sulfur, without aromatic hydrocarbons, not oxygen-containing, NO, row
Put less, the characteristic such as storage stability is good, its Cetane number can be reconciled with mineral diesel in any proportion up to 90～100.Cause
This, with vegetable oil be raw material Hydrogenation for biodiesel, not only can increase derv fuel yield using Renewable resource, if will
Which is spiked in mineral diesel, can also significantly improve the Cetane number of mineral diesel.But, the oxygen content of vegetable oil is high, oxygen matter
Amount fraction about 11% or so, according to the catalyst with magnesium aluminate spinel as carrier, the water generated in hydrogenation process will cause
The activity of catalyst is slow to be declined.Therefore, it should which the catalyst carrier is modified.
The content of the invention
The present invention provides a kind of preparation method of high hydrothermal stability hydrogenation deoxidation catalyst, and the catalyst for preparing adds
Hydrogen deoxy activity and hydrothermal stability are excellent.
The present invention is achieved by the following technical solutions.
The preparation method of high hydrothermal stability hydrogenation deoxidation catalyst, comprises the steps of：
（1）The preparation of magnesium aluminate spinel：It is 1 in molar ratio:2:0.01 weighs magnesium nitrate, aluminum nitrate and cetyl front three respectively
Base ammonium bromide, respectively will be magnesium nitrate, aluminum nitrate and cetyl trimethylammonium bromide molten with the distilled water of 8 times of weight of magnesium nitrate
Solution, mix homogeneously, the pH value for adjusting solution are 10.6；In 80 DEG C of water-baths, mechanical agitation heats 3 h, and 1 h is stood under room temperature；
After drying, grinding, 6 h of roasting at 600 DEG C in muffle furnace is obtained magnesium aluminate spinel；
（2）Prepare shaping carrier：In mass ratio 6：4：0.3 ratio blend step（1）The magnesium aluminate spinel that obtains, aluminium hydroxide
Dry glue and sesbania powder, and the dust technology of mass fraction 3% is added, Jing extruded mouldings, drying, cutting, roasting obtain shaping carrier
MgAl2O4；
（3）Carrying active ingredients prepare hydrogenation deoxidation catalyst：In mass ratio 1:0.25:0.01, by step（2）The molding for obtaining
Carrier, MoO and NiO, citric acid mix homogeneously, stand 12 h under room temperature, 110 DEG C of 3 h of drying in muffle furnace, 500 DEG C of roastings 3
H, that is, be obtained hydrogenation deoxidation catalyst.
Preferably, above-mentioned steps（1）The condition of middle drying is to be dried 4h at 100 DEG C.
Preferably, above-mentioned steps（2）The condition of middle drying is that 3h is dried at 105 DEG C, and the condition of roasting is roasting at 300 DEG C
2h。
Preferably, above-mentioned steps（3）The mol ratio of middle MoO and NiO is 2:5.
Advantages of the present invention：
A kind of preparation method of high hydrothermal stability hydrogenation deoxidation catalyst that the present invention is provided, the aperture of carrier magnesium aluminate spinel
It is larger, the catalyst hydrogenation deoxy activity for preparing and hydrothermal stability it is excellent.
Specific embodiment
Embodiment 1
The preparation method of high hydrothermal stability hydrogenation deoxidation catalyst, comprises the steps of：
（1）The preparation of magnesium aluminate spinel：It is 1 in molar ratio:2:0.01 weighs magnesium nitrate, aluminum nitrate and cetyl front three respectively
Base ammonium bromide, respectively will be magnesium nitrate, aluminum nitrate and cetyl trimethylammonium bromide molten with the distilled water of 8 times of weight of magnesium nitrate
Solution, mix homogeneously, the pH value for adjusting solution are 10.6；In 80 DEG C of water-baths, mechanical agitation heats 3 h, and 1 h is stood under room temperature；
After drying, grinding, 6 h of roasting at 600 DEG C in muffle furnace is obtained magnesium aluminate spinel；
（2）Prepare shaping carrier：In mass ratio 6：4：0.3 ratio blend step（1）The magnesium aluminate spinel that obtains, aluminium hydroxide
Dry glue and sesbania powder, and the dust technology of mass fraction 3% is added, Jing extruded mouldings, drying, cutting, roasting obtain shaping carrier
MgAl2O4；
（3）Carrying active ingredients prepare hydrogenation deoxidation catalyst：In mass ratio 1:0.25:0.01, by step（2）The molding for obtaining
Carrier, MoO and NiO, citric acid mix homogeneously, stand 12 h under room temperature, 110 DEG C of 3 h of drying in muffle furnace, 500 DEG C of roastings 3
H, that is, be obtained hydrogenation deoxidation catalyst.
Above-mentioned steps（1）The condition of middle drying is to be dried 4h at 100 DEG C.
Above-mentioned steps（2）The condition of middle drying is that 3h is dried at 105 DEG C, and the condition of roasting is roasting 2h at 300 DEG C.
Above-mentioned steps（3）The mol ratio of middle MoO and NiO is 2:5.
Claims (4)
1. the preparation method of high hydrothermal stability hydrogenation deoxidation catalyst, it is characterised in that：Comprise the steps of：
（1）The preparation of magnesium aluminate spinel：It is 1 in molar ratio:2:0.01 weighs magnesium nitrate, aluminum nitrate and cetyl front three respectively
Base ammonium bromide, respectively will be magnesium nitrate, aluminum nitrate and cetyl trimethylammonium bromide molten with the distilled water of 8 times of weight of magnesium nitrate
Solution, mix homogeneously, the pH value for adjusting solution are 10.6；In 80 DEG C of water-baths, mechanical agitation heats 3 h, and 1 h is stood under room temperature；
After drying, grinding, 6 h of roasting at 600 DEG C in muffle furnace is obtained magnesium aluminate spinel；
（2）Prepare shaping carrier：In mass ratio 6：4：0.3 ratio blend step（1）The magnesium aluminate spinel that obtains, aluminium hydroxide
Dry glue and sesbania powder, and the dust technology of mass fraction 3% is added, Jing extruded mouldings, drying, cutting, roasting obtain shaping carrier
MgAl2O4；
（3）Carrying active ingredients prepare hydrogenation deoxidation catalyst：In mass ratio 1:0.25:0.01, by step（2）The molding for obtaining
Carrier, MoO and NiO, citric acid mix homogeneously, stand 12 h under room temperature, 110 DEG C of 3 h of drying in muffle furnace, 500 DEG C of roastings 3
H, that is, be obtained hydrogenation deoxidation catalyst.
2. the preparation method of high hydrothermal stability hydrogenation deoxidation catalyst according to claim 1, it is characterised in that：Step
（1）The condition of middle drying is to be dried 4h at 100 DEG C.
3. the preparation method of high hydrothermal stability hydrogenation deoxidation catalyst according to claim 1, it is characterised in that：Step
（2）The condition of middle drying is that 3h is dried at 105 DEG C, and the condition of roasting is roasting 2h at 300 DEG C.
4. the preparation method of high hydrothermal stability hydrogenation deoxidation catalyst according to claim 1, it is characterised in that：Step
（3）The mol ratio of middle MoO and NiO is 2:5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611012129.XA CN106552635A (en) | 2016-11-17 | 2016-11-17 | The preparation method of high hydrothermal stability hydrogenation deoxidation catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611012129.XA CN106552635A (en) | 2016-11-17 | 2016-11-17 | The preparation method of high hydrothermal stability hydrogenation deoxidation catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106552635A true CN106552635A (en) | 2017-04-05 |
Family
ID=58443248
Family Applications (1)
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| CN201611012129.XA Pending CN106552635A (en) | 2016-11-17 | 2016-11-17 | The preparation method of high hydrothermal stability hydrogenation deoxidation catalyst |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942011A (en) * | 2019-03-07 | 2019-06-28 | 昆明理工大学 | A kind of copper load magnesium aluminate nano-powder and preparation method thereof |
| CN110756196A (en) * | 2018-07-26 | 2020-02-07 | 中国石油天然气股份有限公司 | Preparation method of vegetable oil hydrodeoxygenation catalyst |
| CN114522697A (en) * | 2020-11-23 | 2022-05-24 | 中国科学院大连化学物理研究所 | Biological oil hydrodeoxygenation catalyst, preparation and application |
| CN116589363A (en) * | 2023-05-17 | 2023-08-15 | 河南省君恒实业集团生物科技有限公司 | Preparation method of catalyst for preparing 1, 3-cyclohexanediamine by hydrogenating m-xylylenediamine in micro-packed bed |
-
2016
- 2016-11-17 CN CN201611012129.XA patent/CN106552635A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110756196A (en) * | 2018-07-26 | 2020-02-07 | 中国石油天然气股份有限公司 | Preparation method of vegetable oil hydrodeoxygenation catalyst |
| CN110756196B (en) * | 2018-07-26 | 2022-10-04 | 中国石油天然气股份有限公司 | Preparation method of vegetable oil hydrodeoxygenation catalyst |
| CN109942011A (en) * | 2019-03-07 | 2019-06-28 | 昆明理工大学 | A kind of copper load magnesium aluminate nano-powder and preparation method thereof |
| CN114522697A (en) * | 2020-11-23 | 2022-05-24 | 中国科学院大连化学物理研究所 | Biological oil hydrodeoxygenation catalyst, preparation and application |
| CN114522697B (en) * | 2020-11-23 | 2024-02-13 | 中国科学院大连化学物理研究所 | Biological grease hydrodeoxygenation catalyst, preparation and application |
| CN116589363A (en) * | 2023-05-17 | 2023-08-15 | 河南省君恒实业集团生物科技有限公司 | Preparation method of catalyst for preparing 1, 3-cyclohexanediamine by hydrogenating m-xylylenediamine in micro-packed bed |
| CN116589363B (en) * | 2023-05-17 | 2024-05-03 | 河南省君恒实业集团生物科技有限公司 | Preparation method of catalyst for preparing 1, 3-cyclohexanediamine by hydrogenating m-xylylenediamine in micro-packed bed |
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Application publication date: 20170405 |
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