CN110354861A - A kind of catalyst and preparation method thereof for removing alkene - Google Patents
A kind of catalyst and preparation method thereof for removing alkene Download PDFInfo
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- CN110354861A CN110354861A CN201910704349.6A CN201910704349A CN110354861A CN 110354861 A CN110354861 A CN 110354861A CN 201910704349 A CN201910704349 A CN 201910704349A CN 110354861 A CN110354861 A CN 110354861A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 111
- 150000001336 alkenes Chemical class 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 111
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 64
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000654 additive Substances 0.000 claims abstract description 37
- 230000000996 additive effect Effects 0.000 claims abstract description 37
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 32
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 21
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 17
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 90
- 239000000243 solution Substances 0.000 claims description 72
- 238000001035 drying Methods 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 38
- 229910017604 nitric acid Inorganic materials 0.000 claims description 38
- 239000011812 mixed powder Substances 0.000 claims description 26
- 239000011259 mixed solution Substances 0.000 claims description 26
- 241000219782 Sesbania Species 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 238000000465 moulding Methods 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 14
- 229910001593 boehmite Inorganic materials 0.000 claims description 10
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 10
- 239000012752 auxiliary agent Substances 0.000 claims description 9
- 229920000609 methyl cellulose Polymers 0.000 claims description 9
- 239000001923 methylcellulose Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 229920001971 elastomer Polymers 0.000 claims description 5
- 239000000806 elastomer Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 abstract description 20
- 239000010970 precious metal Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 5
- 229930195733 hydrocarbon Natural products 0.000 abstract description 5
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 5
- 229910000510 noble metal Inorganic materials 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 239000004411 aluminium Substances 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 8
- 238000007493 shaping process Methods 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229910000480 nickel oxide Inorganic materials 0.000 description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 5
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000000116 mitigating effect Effects 0.000 description 3
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 3
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 2
- 238000001833 catalytic reforming Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229940078494 nickel acetate Drugs 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000008096 xylene 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
- B01J23/74—Iron group metals
- B01J23/755—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
- 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
- B01J23/83—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 rare earths or actinides
-
- 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
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
-
- 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
- C10G35/00—Reforming naphtha
- C10G35/04—Catalytic reforming
- C10G35/06—Catalytic reforming characterised by the catalyst used
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)
- Catalysts (AREA)
Abstract
The present invention relates to technical field of petrochemical industry more particularly to a kind of catalyst and preparation method thereof for removing alkene.The catalyst includes: 40~90 parts of aluminium oxide according to parts by weight；2~50 parts of nickel；1~20 part of additive；The additive includes one or more of titanium oxide, cerium oxide, lanthana and silica.The catalyst for removing alkene in the present invention is using non-precious metal nickel as active component, and using aluminium oxide as carrier, specific additive adjusts the acid-base property of catalyst；Meanwhile the catalyst that these types of component acts synergistically has been reduced as far as the loss of aromatic hydrocarbons, has improved BTX quality while removing alkene.In addition, conventional selective olefinic hydrocarbon expelling catalyzer is usually all noble metal catalyst, and the catalyst provided by the present invention for removing alkene is non-precious metal catalyst, and effect is good, at low cost.
Description
Technical field
The present invention relates to technical field of petrochemical industry more particularly to a kind of catalyst and its preparation side for removing alkene
Method.
Background technique
Catalytic reforming is important the process of oil product conversion chemicals, is to improve octane number, volume increase aromatic hydrocarbons
Important means.In recent years, with the raising of motor petrol standard, high-grade gasoline becomes the necessity in market.With chemical industry row
The development of industry, application also more and more extensive, BTX (benzene, toluene, the diformazan of high-quality of benzene,toluene,xylene, C9 aromatic hydrocarbons etc.
Benzene) it is the important means for improving the market competitiveness.
During naphtha is reformed, some olefin generation is had, the presence of alkene seriously affects downstream extracting portion
Divide the quality of BTX, and influences the service life of extract.The method of traditional processing alkene is removed using carclazyte, but
Carclazyte easily inactivates, and service life is short, it is frequent to change agent, it usually needs changes once within 2-3 months, when olefin(e) centent is high, carclazyte is used
Service life is shorter, and spent bleaching clay can not regenerate, and dangerous waste processing cost is high, pollutes environment.Afterwards after study, noble metal hydrogenation catalyst
The problems such as having obtained good development, but having needed import mostly there is also at high cost, noble metal, be limited by foreign countries.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing a kind of for removing the catalyst and its system of alkene
Preparation Method, provided by the present invention for remove alkene catalyst while reducing olefin of reforming oil content, can be effective
The loss of aromatic hydrocarbons is controlled, BTX quality is improved.
The present invention provides a kind of for removing the catalyst of alkene, includes: according to parts by weight
40~90 parts of aluminium oxide；
2~50 parts of nickel；
1~20 part of additive；
The additive includes one or more of titanium oxide, cerium oxide, lanthana and silica.
Preferably, the aperture for removing the catalyst of alkene is 6.0~12.0nm；
The specific surface area for removing the catalyst of alkene is 100~300m2/g。
The present invention also provides a kind of for removing the preparation method of the catalyst of alkene, comprising the following steps:
A1 the metal salt of nickel is mixed with solvent), obtains the solution containing active component；The solvent includes water or dust technology
Solution；
B1 carrier is mixed with the solution containing active component), after drying, roasting, obtains catalyst；The carrier
Including aluminium oxide；
Or the following steps are included:
A2) activated alumina, the compound of nickel, additive, auxiliary agent and water are mixed, obtain mixed liquor；
B2 the mixed liquor) is subjected to extruded moulding after drying, roasting and obtains catalyst.
Preferably, step B1) in, the carrier is prepared in accordance with the following methods:
A1) by activated alumina, sesbania powder, methylcellulose and additive according to mass ratio be 91~94:0~6:0~
2:0.5~19 is mixed, and obtains mixed powder；
The additive includes one or more of lanthana, silica, cerium oxide and metatitanic acid；
B1) citric acid, nitric acid solution and water are mixed, obtain mixed solution；
C1) mixed powder and the mixed solution are mixed, after molding, drying, roasting, obtain carrier.
Preferably, the activated alumina is selected from aluminum hydroxide solid elastomer or boehmite；
The activated alumina, citric acid, nitric acid solution and water mass ratio be 91~94:2.5~4.2:1.5~3.5:
60~70；
The mass concentration of the nitric acid solution is 65~67%.
Preferably, step B1) in, the mass ratio of the carrier and the solution containing active component is 1:0.5~1.2.
Preferably, step B1) in, the temperature of the drying is 80~120 DEG C；The temperature of the roasting is 450~550
℃。
Preferably, step A2) in, the activated alumina, the compound of nickel, additive, auxiliary agent and water mass ratio be
84~88:25~32:20~45:12~16:60~70.
Preferably, step A2) in, the auxiliary agent includes one in nitric acid solution, citric acid, sesbania powder and methylcellulose
Kind is several；
The additive includes one or more of cerium oxide, lanthana, metatitanic acid and silica.
Preferably, step B2) in, the temperature of the drying is 80~120 DEG C；The temperature of the roasting is 450~550
℃。
The present invention provides a kind of for removing the catalyst of alkene, according to parts by weight includes: 40~90 parts of aluminium oxide；
2~50 parts of nickel；1~20 part of additive；The additive include one of titanium oxide, cerium oxide, lanthana and silica or
It is several.The catalyst for removing alkene in the present invention is special using aluminium oxide as carrier using non-precious metal nickel as active component
Fixed additive adjusts the acid-base property of catalyst；Meanwhile the catalyst that these types of component acts synergistically is in removing alkene
Meanwhile it being reduced as far as the loss of aromatic hydrocarbons, improve BTX quality.In addition, conventional selective olefinic hydrocarbon expelling catalyzer is usual
It is all noble metal catalyst, and the catalyst provided by the present invention for removing alkene is non-precious metal catalyst, effect is good, at
This is low.
The experimental results showed that it is prepared by the present invention for remove alkene catalyst can under the reaction condition of mitigation,
The olefin(e) centent in reformed oil is effectively reduced, the conversion ratio of alkene is not less than 91.5%；And aromatic hydrocarbons can be lost and be reduced to
Within target value, the loss late of aromatic hydrocarbons is not higher than 0.8%；Catalyst effect is obvious, ensure that the quality of downstream aromatic hydrocarbon product.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
The present invention provides a kind of for removing the catalyst of alkene, includes: according to parts by weight
40~90 parts of aluminium oxide；
2~50 parts of nickel；
1~20 part of additive；
The additive includes one or more of titanium oxide, cerium oxide, lanthana and silica.
Catalyst provided by the present invention for removing alkene includes aluminium oxide.The parts by weight of the aluminium oxide be 40~
90 parts.In certain embodiments of the present invention, the parts by weight of the aluminium oxide be 87 parts, 90 parts, 73.5 parts, 46 parts, 54 parts,
84 parts, 50 parts or 40 parts.
Catalyst provided by the present invention for removing alkene further includes active component nickel.The parts by weight of the nickel are 2
~50 parts.In certain embodiments of the present invention, the parts by weight of the nickel be 2 parts, 5 parts, 15 parts, 50 parts, 28 parts, 30 parts,
12 parts or 25 parts.
Catalyst provided by the present invention for removing alkene further includes additive.The parts by weight of the additive are 1
~20 parts.In certain embodiments of the present invention, the parts by weight of the additive be 1 part, 8 parts, 11.5 parts, 4 parts, 18 parts,
20 parts or 35 parts.The additive is used to adjust the acid-base property of catalyst.The additive includes titanium oxide, cerium oxide, oxidation
One or more of lanthanum and silica.
The catalyst for removing alkene in the present invention is to carry with aluminium oxide using non-precious metal nickel as active component
Body, specific additive adjust the acid-base property of catalyst；Meanwhile the catalyst that these types of component acts synergistically is in removing alkene
While hydrocarbon, it has been reduced as far as the loss of aromatic hydrocarbons, has improved BTX quality.
In an embodiment of the present invention, the aperture for removing the catalyst of alkene is 6.0~12.0nm.Certain
In embodiment, it is described for remove alkene catalyst aperture be 7.9nm, 8.6nm, 8.3nm, 10.0nm, 9.7nm,
8.7nm, 6.3nm or 6.0nm.In an embodiment of the present invention, the specific surface area for removing the catalyst of alkene is 100
~300m2/g.In certain embodiments, the specific surface area for removing the catalyst of alkene is 190m2/g、183m2/g、
201m2/g、230m2/g、205m2/g、261m2/g、142m2/ g or 129m2/g。
Catalyst provided by the invention is for the generation oil after catalytic reforming, while removing alkene, as far as possible
Ground reduces the loss of aromatic hydrocarbons, improves BTX quality.In addition, the selective olefinic hydrocarbon expelling catalyzer of market is usually all precious metal catalyst
Agent, and the catalyst provided by the present invention for removing alkene is non-precious metal catalyst, effect is good, at low cost.
The present invention also provides the preparation methods of the catalyst described above for removing alkene, and the preparation method can
Think infusion process.Specifically, the following steps are included:
A1 the metal salt of nickel is mixed with solvent), obtains the solution containing active component；The solvent includes water or dust technology
Solution；
B1 carrier is mixed with the solution containing active component), after drying, roasting, obtains catalyst；The carrier
Including aluminium oxide.
In certain embodiments of the present invention, step A1) specifically:
By the dissolving metal salts of nickel into solvent, the solution containing active component is obtained；The solvent includes water or dust technology
Solution.
In certain embodiments of the present invention, the metal salt of the nickel includes nickelous carbonate, nickel acetate, nickel nitrate or oxidation
Nickel.
In certain embodiments, the mass concentration of the dilute nitric acid solution is 8~12%.In certain embodiments, described
The mass concentration of dilute nitric acid solution is 10%.
In an embodiment of the present invention, the carrier is prepared in accordance with the following methods:
A1) by activated alumina, sesbania powder, methylcellulose and additive according to mass ratio be 91~94:0~6:0~
2:0.5~19 is mixed, and obtains mixed powder；
The additive includes one or more of lanthana, silica, cerium oxide and metatitanic acid；
B1) citric acid, nitric acid solution and water are mixed, obtain mixed solution；
C1) mixed powder and the mixed solution are mixed, after molding, drying, roasting, obtain carrier.
In certain embodiments of the present invention, the activated alumina is selected from aluminum hydroxide solid elastomer or boehmite.
In certain embodiments of the present invention, the specific surface area of the activated alumina is 100~350m2/g.Certain
In embodiment, the specific surface area of the activated alumina is 210m2/g、195m2/g、232m2/g、248m2/g、214m2/g、
273m2/g、196m2/ g or 240m2/g。
In certain embodiments of the present invention, the quality of the activated alumina, sesbania powder, methylcellulose and additive
Than for 93.5:2:0:0.64,92.5:2:0:4.93,91.5:3:0:8.59,94:0:2:4.9,93.7:2:0:18.74 or
93.5:2:0:2.67.
In certain embodiments of the present invention, the mass ratio of the activated alumina, citric acid, nitric acid solution and water is 91
~94:2.5~4.2:1.5~3.5:60~70.In certain embodiments, the activated alumina, citric acid, nitric acid solution and
The mass ratio of water is 93.5:2.5:2:65,92.5:2.5:3:62,91.5:2.5:3:67,94:2.5:1.5:70 or 94:2.5:
1.8:60.
In certain embodiments of the present invention, the mass concentration of the nitric acid solution is 65~67%.
It in certain embodiments of the present invention, further include shaping after the molding.
In certain embodiments of the present invention, the temperature of the drying is 100~120 DEG C.In certain embodiments, described
The temperature of drying is 120 DEG C or 100 DEG C.In certain embodiments of the present invention, the time of the drying is 6~10h.Certain
In embodiment, the time of the drying is 6h, 8h, 10h.
In certain embodiments of the present invention, the temperature of the roasting is 450~550 DEG C.In certain embodiments, described
The temperature of roasting is 480 DEG C, 550 DEG C, 540 DEG C, 500 DEG C or 520 DEG C.In certain embodiments of the present invention, the roasting
Time is 4~6h.In certain embodiments, the time of the roasting is 5h, 4h, 6h.
After obtaining carrier, carrier is mixed with the solution containing active component, after drying, roasting, obtains catalyst.
In certain embodiments of the present invention, the mass ratio of the carrier and the solution containing active component is 1:0.5
~1.5.In certain embodiments, the mass ratio of the carrier and the solution containing active component is 1:0.65,1:0.55,1:
0.70 or 1:0.71.
In certain embodiments of the present invention, the temperature of the drying is 80~120 DEG C.In certain embodiments, described
The temperature of drying is 80 DEG C, 100 DEG C or 120 DEG C.In certain embodiments of the present invention, the time of the drying is 6~10h.
In certain embodiments, the time of the drying is 10h, 8h or 6h.
In certain embodiments of the present invention, the temperature of the roasting is 450~550 DEG C.In certain embodiments, described
The temperature of roasting is 450 DEG C, 480 DEG C, 500 DEG C or 530 DEG C.In certain embodiments of the present invention, the time of the roasting is 4
~6h.In certain embodiments, the time of the roasting is 4h, 5h or 6h.
In the present invention, the preparation method of the catalyst for removing alkene can also be kneading method.Specifically, including
Following steps:
A2) activated alumina, the compound of nickel, additive, auxiliary agent and water are mixed, obtain mixed liquor；
B2 the mixed liquor) is subjected to extruded moulding after drying, roasting and obtains catalyst.
In certain embodiments of the present invention, the activated alumina is selected from aluminum hydroxide solid elastomer or boehmite.
In certain embodiments of the present invention, the specific surface area of the activated alumina is 100~350m2/g。
In certain embodiments of the present invention, the matter of the activated alumina, the compound of nickel, additive, auxiliary agent and water
Amount is than being 84~88:25~32:20~45:12~16:60~70.
In certain embodiments of the present invention, the compound of the nickel includes nickel oxide or nickelous carbonate.In certain of the invention
In a little embodiments, the additive includes one or more of cerium oxide, lanthana, metatitanic acid and silica.The auxiliary agent
Including one or more of nitric acid solution, citric acid, sesbania powder and methylcellulose.
In certain embodiments of the present invention, the step A2) specifically:
A2) activated alumina, the compound of nickel, sesbania powder, silica and metatitanic acid are mixed, obtain mixed powder；
B2) citric acid, nitric acid solution and water are mixed, obtain mixed solution；
C2) mixed powder and mixed solution are mixed, obtain mixed liquor.
In certain embodiments, the quality of the activated alumina, the compound of nickel, sesbania powder, silica and metatitanic acid
Than for 87.5:31.50:6:6.30:14.70.
In certain embodiments of the present invention, the mass concentration of the nitric acid solution is 65~67%.
In certain embodiments of the present invention, the mass ratio of the activated alumina, citric acid, nitric acid solution and water is
87.5:3.5:3:65.
In certain embodiments of the present invention, after the mixed liquor being carried out extruded moulding, the temperature of the drying is
80~120 DEG C.In certain embodiments, the temperature of the drying is 120 DEG C.The time of the drying is 6~8h.In certain realities
It applies in example, the time of the drying is 6h.The temperature of the roasting is 500~550 DEG C.In certain embodiments, the roasting
Temperature be 540 DEG C.The time of the roasting is 4~6h.In certain embodiments, the time of the roasting is 4h.
In certain embodiments of the present invention, the step A2) specifically:
A2) activated alumina, nickel oxide, sesbania powder, silica and metatitanic acid are mixed, obtain mixed powder；
B2) citric acid, nitric acid solution and water are mixed, obtain mixed solution；
C2) mixed powder and mixed solution are mixed, obtain mixed liquor.
In certain embodiments, the mass ratio by activated alumina, nickel oxide, sesbania powder, silica and metatitanic acid
For 87.5:31.50:6:6.30:14.70.
In certain embodiments of the present invention, the mass concentration of the nitric acid solution is 65~67%.
In certain embodiments of the present invention, the mass ratio of the activated alumina, citric acid, nitric acid solution and water is
87.5:3.5:3:65.
In certain embodiments of the present invention, after the mixed liquor being carried out extruded moulding, the temperature of the drying is
80~120 DEG C.In certain embodiments, the temperature of the drying is 120 DEG C.The time of the drying is 6~8h.In certain realities
It applies in example, the time of the drying is 6h.The temperature of the roasting is 500~550 DEG C.In certain embodiments, the roasting
Temperature be 540 DEG C.The time of the roasting is 4~6h.In certain embodiments, the time of the roasting is 4h.
The present invention has no special limitation to the source of the raw material used above, can be general commercially available.
The present invention provides a kind of for removing the catalyst of alkene, according to parts by weight includes: 40~90 parts of aluminium oxide；
2~50 parts of nickel；1~20 part of additive；The additive include one of titanium oxide, cerium oxide, lanthana and silica or
It is several.The catalyst for removing alkene in the present invention is special using aluminium oxide as carrier using non-precious metal nickel as active component
Fixed additive adjusts the acid-base property of catalyst；Meanwhile the catalyst that these types of component acts synergistically is in removing alkene
Meanwhile it being reduced as far as the loss of aromatic hydrocarbons, improve BTX quality.In addition, conventional selective olefinic hydrocarbon expelling catalyzer is usual
It is all noble metal catalyst, and the catalyst provided by the present invention for removing alkene is non-precious metal catalyst, effect is good, at
This is low.
The experimental results showed that it is prepared by the present invention for remove alkene catalyst can under the reaction condition of mitigation,
The olefin(e) centent in reformed oil is effectively reduced, the conversion ratio of alkene is not less than 91.5%；And aromatic hydrocarbons can be lost and be reduced to
Within target value, the loss late of aromatic hydrocarbons is not higher than 0.8%；Catalyst effect is obvious, ensure that the quality of downstream aromatic hydrocarbon product.
In order to further illustrate the present invention, it a kind of is urged for removing alkene below with reference to embodiment to provided by the invention
Agent and preparation method thereof is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Raw material used in following embodiment is general commercially available.
Embodiment 1
It is a kind of for removing the catalyst of alkene, include: according to parts by weight
87 parts of aluminium oxide；
12 parts of nickel；
1 part of cerium oxide；
The preparation method of the catalyst includes:
1, carrier is prepared:
By activated alumina, sesbania powder and cerium oxide according to mass ratio be 93.5:2:0.64 mix, obtain mixed powder；
The activated alumina is selected from aluminum hydroxide solid elastomer；The specific surface area of the activated alumina is 210m2/g；
Citric acid, the nitric acid solution that mass concentration is 65% and water are mixed, mixed solution is obtained；The active oxidation
Aluminium, citric acid, nitric acid solution and water mass ratio be 93.5:2.5:2:65；
The mixed powder and the mixed solution are mixed, roasted in 120 DEG C of drying 6h at 480 DEG C through molding, shaping
After burning 5h, carrier is obtained.
2, nickelous carbonate is dissolved in the dilute nitric acid solution that mass concentration is 10%, obtains the solution containing active component.
3, the solution containing active component is impregnated on carrier, is obtained after 450 DEG C of roasting 4h in 80 DEG C of drying 10h
To catalyst；The mass ratio of the carrier and the solution containing active component is 1:0.65.
Through detecting, the aperture of the catalyst is 7.9nm；The specific surface area of the catalyst is 190m2/g。
Embodiment 2
It is a kind of for removing the catalyst of alkene, include: according to parts by weight
The preparation method of the catalyst includes:
1, carrier is prepared:
By activated alumina, sesbania powder, cerium oxide and lanthana according to mass ratio be 92.5:2:1.23:3.70 mix, obtain
To mixed powder；The activated alumina is selected from boehmite；The specific surface area of the activated alumina is 195m2/g；
Citric acid, the nitric acid solution that mass concentration is 65% and water are mixed, mixed solution is obtained；The active oxidation
Aluminium, citric acid, nitric acid solution and water mass ratio be 92.5:2.5:3:62；
The mixed powder and the mixed solution are mixed, roasted in 120 DEG C of drying 6h at 550 DEG C through molding, shaping
After burning 4h, carrier is obtained.
2, nickel acetate is dissolved in deionized water, obtains the solution containing active component.
3, the solution containing active component is impregnated on carrier, is obtained after 480 DEG C of roasting 5h in 100 DEG C of drying 8h
To catalyst；The mass ratio of the carrier and the solution containing active component is 1:0.55.
Through detecting, the aperture of the catalyst is 8.6nm；The specific surface area of the catalyst is 183m2/g。
Embodiment 3
It is a kind of for removing the catalyst of alkene, include: according to parts by weight
The preparation method of the catalyst includes:
1, carrier is prepared:
By activated alumina, sesbania powder, lanthana and metatitanic acid according to mass ratio be 91.5:3:1.12:7.47 mix, obtain
To mixed powder；The activated alumina is selected from boehmite；The specific surface area of the activated alumina is 232m2/g；
Citric acid, the nitric acid solution that mass concentration is 65% and water are mixed, mixed solution is obtained；The active oxidation
Aluminium, citric acid, nitric acid solution and water mass ratio be 91.5:2.5:3:67；
The mixed powder and the mixed solution are mixed, roasted in 120 DEG C of drying 8h at 540 DEG C through molding, shaping
After burning 6h, carrier is obtained.
2, nickel nitrate is dissolved in deionized water, obtains the solution containing active component.
3, the solution containing active component is impregnated on carrier, is obtained after 500 DEG C of roasting 4h in 100 DEG C of drying 8h
To catalyst；The mass ratio of the carrier and the solution containing active component is 1:0.70.
Through detecting, the aperture of the catalyst is 8.3nm；The specific surface area of the catalyst is 201m2/g。
Embodiment 4
It is a kind of for removing the catalyst of alkene, include: according to parts by weight
46 parts of aluminium oxide；
50 parts of nickel；
4 parts of silica；
The preparation method of the catalyst includes:
1, carrier is prepared:
By activated alumina, methylcellulose, silica according to mass ratio be 94:2:4.9 mix, obtain mixed powder；
The activated alumina is selected from boehmite；The specific surface area of the activated alumina is 248m2/g；
Citric acid, the nitric acid solution that mass concentration is 65% and water are mixed, mixed solution is obtained；The active oxidation
Aluminium, citric acid, nitric acid solution and water mass ratio be 94:2.5:1.5:70；
The mixed powder and the mixed solution are mixed, roasted in 100 DEG C of drying 10h at 500 DEG C through molding, shaping
After burning 4h, carrier is obtained.
2, nickel nitrate is dissolved in deionized water, obtains the solution containing active component.
3, the solution containing active component is impregnated on carrier, in 100 DEG C of drying 10h, after 480 DEG C of roasting 6h,
Obtain catalyst；The mass ratio of the carrier and the solution containing active component is 1:1.03.
Through detecting, the aperture of the catalyst is 10.0nm；The specific surface area of the catalyst is 230m2/g。
Embodiment 5
It is a kind of for removing the catalyst of alkene, include: according to parts by weight
54 parts of aluminium oxide；
28 parts of nickel；
18 parts of titanium oxide；
The preparation method of the catalyst includes:
1, carrier is prepared:
By activated alumina, sesbania powder, metatitanic acid according to mass ratio be 93.7:2:18.74 mix, obtain mixed powder；
The activated alumina is selected from boehmite；The specific surface area of the activated alumina is 214m2/g；
Citric acid, the nitric acid solution that mass concentration is 65% and water are mixed, mixed solution is obtained；The active oxidation
Aluminium, citric acid, nitric acid solution and water mass ratio be 94:2.5:1.8:60；
The mixed powder and the mixed solution are mixed, roasted in 100 DEG C of drying 10h at 520 DEG C through molding, shaping
After burning 4h, carrier is obtained.
2, nickel nitrate is dissolved in deionized water, obtains the solution containing active component.
3, the solution containing active component is impregnated on carrier, is obtained after 500 DEG C of roasting 4h in 100 DEG C of drying 8h
To catalyst；The mass ratio of the carrier and the solution containing active component is 1:0.92.
Through detecting, the aperture of the catalyst is 9.7nm；The specific surface area of the catalyst is 205m2/g。
Embodiment 6
It is a kind of for removing the catalyst of alkene, include: according to parts by weight
84 parts of aluminium oxide；
12 parts of nickel；
4 parts of lanthana；
The preparation method of the catalyst includes:
1, carrier is prepared:
By activated alumina, sesbania powder, lanthana according to mass ratio be 93.5:2:2.67 mix, obtain mixed powder；Institute
It states activated alumina and is selected from boehmite；The specific surface area of the activated alumina is 273m2/g；
Citric acid, the nitric acid solution that mass concentration is 65% and water are mixed, mixed solution is obtained；The active oxidation
Aluminium, citric acid, nitric acid solution and water mass ratio be 93.5:2.5:2:65；
The mixed powder and the mixed solution are mixed, roasted in 100 DEG C of drying 8h at 550 DEG C through molding, shaping
After burning 4h, carrier is obtained.
2, nickel nitrate is dissolved in deionized water, obtains the solution containing active component.
3, the solution containing active component is impregnated on carrier, is obtained after 530 DEG C of roasting 6h in 120 DEG C of drying 6h
To catalyst；The mass ratio of the carrier and the solution containing active component is 1:0.71.
Through detecting, the aperture of the catalyst is 8.7nm；The specific surface area of the catalyst is 261m2/g。
Embodiment 7
It is a kind of for removing the catalyst of alkene, include: according to parts by weight
The preparation method of the catalyst includes:
By activated alumina, nickel oxide, sesbania powder, silica and metatitanic acid according to mass ratio be 87.5:31.50:6:
6.30:14.70 mixing, mixed powder is obtained；The activated alumina is selected from boehmite；The ratio table of the activated alumina
Area is 196m2/g；
Citric acid, the nitric acid solution that mass concentration is 65% and water are mixed, mixed solution is obtained；The active oxidation
Aluminium, citric acid, nitric acid solution and water mass ratio be 87.5:3.5:3:65；
The mixed powder and mixed solution are mixed, mixed liquor is obtained；
The mixed liquor is subjected to extruded moulding, obtains catalyst after 540 DEG C of roasting 4h in 120 DEG C of drying 6h.
Through detecting, the aperture of the catalyst is 6.3nm；The specific surface area of the catalyst is 142m2/g。
Embodiment 8
It is a kind of for removing the catalyst of alkene, include: according to parts by weight
The preparation method of the catalyst includes:
By activated alumina, nickel oxide, methylcellulose, sesbania powder, silica, metatitanic acid, cerium oxide according to mass ratio
For 84.3:31.61:2:6:10.12:13.91:20.23 mixing, mixed powder is obtained；The activated alumina, which is selected from, intends thin water
Aluminium stone；The specific surface area of the activated alumina is 240m2/g；
Citric acid, the nitric acid solution that mass concentration is 65% and water are mixed, mixed solution is obtained；The active oxidation
Aluminium, citric acid, nitric acid solution and water mass ratio be 84.3:4.2:3.5:65；
The mixed powder and mixed solution are mixed, mixed liquor is obtained；
The mixed liquor is subjected to extruded moulding, obtains catalyst after 540 DEG C of roasting 4h in 120 DEG C of drying 6h.
Through detecting, the aperture of the catalyst is 6.0nm；The specific surface area of the catalyst is 129m2/g。
Embodiment 9
Catalyst made from Examples 1 to 8 is carried out to the evaluation of catalyst on fixed bed simulator, catalysis before evaluating
Agent is through overactivation.Raw material is oily using CONTINUOUS REFORMER generation, and 90 DEG C of temperature, pressure 0.5MPa, hydrogen-oil ratio 50:1, volume space velocity 8h-1,
After simulator normal operation, for 24 hours when sampling and testing product in alkene and arene content, calculate olefin conversion and aromatic hydrocarbons damage
Mistake rate.The results are shown in Table 1.
The Evaluation results of catalyst made from 1 Examples 1 to 8 of table
| Number | Olefin conversion % | Aromatic hydrocarbons loss late/% |
| Embodiment 1 | 91.5 | 0.1 |
| Embodiment 2 | 96.4 | 0.4 |
| Embodiment 3 | 99.2 | 0.2 |
| Embodiment 4 | 99.3 | 0.8 |
| Embodiment 5 | 98.9 | 0.1 |
| Embodiment 6 | 97.5 | 0.3 |
| Embodiment 7 | 98.3 | 0.7 |
| Embodiment 8 | 97.9 | 0.5 |
As it can be seen from table 1 it is prepared by the present invention for remove alkene catalyst can under the reaction condition of mitigation,
The olefin(e) centent in reformed oil is effectively reduced, the conversion ratio of alkene is not less than 91.5%；And aromatic hydrocarbons can be lost and be reduced to
Within target value, the loss late of aromatic hydrocarbons is not higher than 0.8%；Catalyst effect is obvious, ensure that the quality of downstream aromatic hydrocarbon product.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (10)
1. a kind of for removing the catalyst of alkene, which is characterized in that include: according to parts by weight
40~90 parts of aluminium oxide；
2~50 parts of nickel；
1~20 part of additive；
The additive includes one or more of titanium oxide, cerium oxide, lanthana and silica.
2. catalyst according to claim 1, which is characterized in that the aperture of the catalyst for removing alkene is
6.0~12.0nm；
The specific surface area for removing the catalyst of alkene is 100~300m2/g。
3. a kind of for removing the preparation method of the catalyst of alkene, comprising the following steps:
A1 the metal salt of nickel is mixed with solvent), obtains the solution containing active component；The solvent includes that water or dust technology are molten
Liquid；
B1 carrier is mixed with the solution containing active component), after drying, roasting, obtains catalyst；The carrier includes
Aluminium oxide；
Or the following steps are included:
A2) activated alumina, the compound of nickel, additive, auxiliary agent and water are mixed, obtain mixed liquor；
B2 the mixed liquor) is subjected to extruded moulding after drying, roasting and obtains catalyst.
4. preparation method according to claim 3, which is characterized in that step B1) in, the carrier in accordance with the following methods into
Row preparation:
It a1 is) 91~94:0~6:0~2:0.5 according to mass ratio by activated alumina, sesbania powder, methylcellulose and additive
~19 mix, and obtain mixed powder；
The additive includes one or more of lanthana, silica, cerium oxide and metatitanic acid；
B1) citric acid, nitric acid solution and water are mixed, obtain mixed solution；
C1) mixed powder and the mixed solution are mixed, after molding, drying, roasting, obtain carrier.
5. the preparation method according to claim 4, which is characterized in that the activated alumina be selected from aluminum hydroxide solid elastomer or
Boehmite；
The activated alumina, citric acid, nitric acid solution and water mass ratio be 91~94:2.5~4.2:1.5~3.5:60~
70；
The mass concentration of the nitric acid solution is 65~67%.
6. preparation method according to claim 3, which is characterized in that step B1) in, the carrier contains active group with described
The mass ratio of the solution divided is 1:0.5~1.2.
7. preparation method according to claim 3, which is characterized in that step B1) in, the temperature of the drying is 80~
120℃；The temperature of the roasting is 450~550 DEG C.
8. preparation method according to claim 3, which is characterized in that step A2) in, the change of the activated alumina, nickel
The mass ratio for closing object, additive, auxiliary agent and water is 84~88:25~32:20~45:12~16:60~70.
9. preparation method according to claim 3, which is characterized in that step A2) in, the auxiliary agent include nitric acid solution,
One or more of citric acid, sesbania powder and methylcellulose；
The additive includes one or more of cerium oxide, lanthana, metatitanic acid and silica.
10. preparation method according to claim 3, which is characterized in that step B2) in, the temperature of the drying is 80~
120℃；The temperature of the roasting is 450~550 DEG C.
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