CN105032474A - Supported nanometer metal catalyst used for 1-butene and production through C4 distillate cracking - Google Patents
Supported nanometer metal catalyst used for 1-butene and production through C4 distillate cracking Download PDFInfo
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- CN105032474A CN105032474A CN201510270390.9A CN201510270390A CN105032474A CN 105032474 A CN105032474 A CN 105032474A CN 201510270390 A CN201510270390 A CN 201510270390A CN 105032474 A CN105032474 A CN 105032474A
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- catalyst
- cracking
- roasting
- metal catalyst
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- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- 238000005336 cracking Methods 0.000 title claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 15
- 239000002184 metal Substances 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title abstract description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 title abstract 6
- 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 24
- 239000004927 clay Substances 0.000 claims abstract description 8
- 239000002808 molecular sieve Substances 0.000 claims abstract description 8
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000010941 cobalt Substances 0.000 claims abstract description 3
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 3
- 230000002860 competitive effect Effects 0.000 claims abstract description 3
- 239000000306 component Substances 0.000 claims abstract description 3
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 239000011733 molybdenum Substances 0.000 claims abstract description 3
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 239000010937 tungsten Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 13
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 claims description 13
- 238000002803 maceration Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005984 hydrogenation reaction Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- -1 wash 3 times Substances 0.000 claims description 3
- 239000002156 adsorbate Substances 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000003463 adsorbent Substances 0.000 abstract 1
- 238000011284 combination treatment Methods 0.000 abstract 1
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
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- Catalysts (AREA)
Abstract
The present invention discloses a supported nanometer metal catalyst used for 1-butene and production through C4 distillate cracking, and relates to the technical field of chemical industry separation, wherein a ZSM-5 molecular sieve is adopted as a carrier, clay is adopted as an adhesive, iron, cobalt, nickel or oxides thereof are adopted as main active components, molybdenum, tungsten or oxides thereof are adopted as auxiliary active components, and citric acid is adopted as a competitive adsorbent. According to the present invention, the match use of the main active components and the auxiliary active components is used, and the dipping method and ultrasound and microwave combination treatment is used, such that the loading rate and the catalysis activity of the catalyst can be improved; and the prepared catalyst has characteristics of good selectivity, high catalysis efficiency and 1-butene yield increasing.
Description
Technical field:
The present invention relates to technical field of chemical separation, be specifically related to a kind of cracking c_4 cut and produce 1-butylene load-type nanometer metal catalyst.
Background technology:
When hydrocarbon cracking production ethene, propylene, the C_4 hydrocarbon of by-product, becomes cracking c_4 cut traditionally, and its content and composition are subject to the impact of cracking stock and process conditions two aspect.Usually when cracking naphtha or diesel oil, the C-4-fraction of by-product is the 8-10% of raw material gross weight, and be characterized in that the content of alkene and alkadienes is up to 92-95%, wherein the content of butadiene is 40-50%.
In order to make full use of the C-4-fraction of by-product, the raw material of some polymerisation can be it can be used as, but require that the content of butadiene in raw material olefin is lower than 1 × 10
-6, therefore need selec-tive hydrogenation butadiene to be converted into 1-butylene or 2-butylene.Need to use catalyst in this hydrogenation reaction, and require that catalyst has good selective and catalytic efficiency.The cracking c_4 cut of our company's exploitation produces the feature that 1-butylene load type metal catalyst has selective good, catalytic efficiency and repeatedly recycles, and has immeasurable application prospect.
Summary of the invention:
Technical problem to be solved by this invention is to provide a kind of selective good and the cracking c_4 cut that catalytic efficiency is high produces 1-butylene load-type nanometer metal catalyst.
Technical problem to be solved by this invention adopts following technical scheme to realize:
A kind of cracking c_4 cut produces 1-butylene load-type nanometer metal catalyst, take ZSM-5 molecular sieve as carrier, clay is binding agent, iron, cobalt, nickel metal or its oxide are main active component, molybdenum, tungsten or its oxide are for helping active component, citric acid is competitive adsorbate, and concrete preparation method is as follows:
(1) help active component to be dispersed in 50-60 part deionized water main for 12-15 part active component and 5-8 part, make maceration extract;
(2) by 80-90 part ZSM-5 molecular sieve dry 8-12h at 70-80 DEG C, then join in maceration extract prepared by step (1), add 8-10 part clay and 3-5 part citric acid again, fully mix, microwave treatment 20-30min at ultrasonic process 15-20min, 65-70 DEG C at 35-45 DEG C;
(3) solution after step (2) being processed filters, and filter residue is through 100-110 DEG C of dry 2-3h, and 450 DEG C of roasting 2-3h, 650 DEG C of roasting 4-5h, obtain final catalyst.
Its using method is: joined by final catalyst in cracking c_4 cut and carry out hydrogenation reaction, reaction terminate after from solution filtering catalyst, wash 3 times, ethanol washes 3 times, again after vacuum drying in 450 DEG C of roasting 2-3h, 650 DEG C of roasting 4-5h, namely can be recycled, access times are 3-5 time.
Described supersonic frequency is 28KHz, and ultrasonic power is 300W/m
2, microwave frequency is 2450MHz, and microwave power is 400W.
The invention has the beneficial effects as follows:
(1) main active component and help active component with the use of, contribute to improving the load factor of catalyst and catalytic activity;
(2) infusion process and ultrasonic wave, microwave in conjunction with process, be conducive to the load factor of raising two kinds of active components;
(3) this catalyst uses by filtration, drying, activation Posterior circle after using, not only environmental protection, and can reduce costs input;
(4) this catalyst has selective good, feature that catalytic efficiency is high, can improve the output of 1-butylene.
Detailed description of the invention:
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with specific embodiment, setting forth the present invention further.
Embodiment 1
A kind of cracking c_4 cut produces 1-butylene load-type nanometer metal catalyst, and preparation method is as follows:
(1) 12g iron powder and 5g molybdenum oxide are dispersed in 50g deionized water, make maceration extract;
(2) by 80gZSM-5 molecular sieve dry 12h at 70-80 DEG C, then join in maceration extract prepared by step (1), then add 8g clay and 3g citric acid, fully mix, microwave treatment 25min at ultrasonic process 15min, 65-70 DEG C at 35-45 DEG C;
(3) solution after step (2) being processed filters, and filter residue is through 100-110 DEG C of dry 3h, and 450 DEG C of roasting 3h, 650 DEG C of roasting 5h, obtain final catalyst.
Its using method is: joined by final catalyst in cracking c_4 cut and carry out hydrogenation reaction, after reaction terminates from solution filtering catalyst, wash 3 times, ethanol washes 3 times, then in 450 DEG C of roasting 3h after vacuum drying, 650 DEG C of roasting 5h, namely can be recycled.
Embodiment 2
A kind of cracking c_4 cut produces 1-butylene load-type nanometer metal catalyst, and preparation method is as follows:
(1) 15g nickel powder and 5g molybdenum oxide are dispersed in 60g deionized water, make maceration extract;
(2) by 80gZSM-5 molecular sieve dry 12h at 70-80 DEG C, then join in maceration extract prepared by step (1), then add 8g clay and 3g citric acid, fully mix, microwave treatment 25min at ultrasonic process 15min, 65-70 DEG C at 35-45 DEG C;
(3) solution after step (2) being processed filters, and filter residue is through 100-110 DEG C of dry 3h, and 450 DEG C of roasting 3h, 650 DEG C of roasting 5h, obtain final catalyst.
The using method of catalyst described in the present embodiment is with embodiment 1.
Embodiment 3
A kind of cracking c_4 cut produces 1-butylene load-type nanometer metal catalyst, and preparation method is as follows:
(1) 15g cobalt oxide and 6g molybdenum oxide are dispersed in 60g deionized water, make maceration extract;
(2) by 90gZSM-5 molecular sieve dry 12h at 70-80 DEG C, then join in maceration extract prepared by step (1), then add 10g clay and 5g citric acid, fully mix, microwave treatment 25min at ultrasonic process 15min, 65-70 DEG C at 35-45 DEG C;
(3) solution after step (2) being processed filters, and filter residue is through 100-110 DEG C of dry 3h, and 450 DEG C of roasting 3h, 650 DEG C of roasting 5h, obtain final catalyst.
The using method of catalyst described in the present embodiment is with embodiment 1.
More than show and describe general principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (3)
1. a cracking c_4 cut produces 1-butylene load-type nanometer metal catalyst, it is characterized in that: take ZSM-5 molecular sieve as carrier, clay is binding agent, iron, cobalt, nickel metal or its oxide are main active component, molybdenum, tungsten or its oxide are for helping active component, citric acid is competitive adsorbate, and concrete preparation method is as follows:
(1) help active component to be dispersed in 50-60 part deionized water main for 12-15 part active component and 5-8 part, make maceration extract;
(2) by 80-90 part ZSM-5 molecular sieve dry 8-12h at 70-80 DEG C, then join in maceration extract prepared by step (1), add 8-10 part clay and 3-5 part citric acid again, fully mix, microwave treatment 20-30min at ultrasonic process 15-20min, 65-70 DEG C at 35-45 DEG C;
(3) solution after step (2) being processed filters, and filter residue is through 100-110 DEG C of dry 2-3h, and 450 DEG C of roasting 2-3h, 650 DEG C of roasting 4-5h, obtain final catalyst.
2. cracking c_4 cut according to claim 1 produces 1-butylene load-type nanometer metal catalyst, and it is characterized in that: described supersonic frequency is 28KHz, ultrasonic power is 300W/m
2, microwave frequency is 2450MHz, and microwave power is 400W.
3. cracking c_4 cut according to claim 1 produces 1-butylene load-type nanometer metal catalyst, it is characterized in that, the using method of described final catalyst is: joined by final catalyst in cracking c_4 cut and carry out hydrogenation reaction, reaction terminate after from solution filtering catalyst, wash 3 times, ethanol washes 3 times, then in 450 DEG C of roasting 2-3h after vacuum drying, 650 DEG C of roasting 4-5h, namely can be recycled, access times are 3-5 time.
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| CN201510270390.9A CN105032474B (en) | 2015-05-25 | 2015-05-25 | A kind of cracking c_4 cut produces 1 butylene load-type nanometer metal catalyst |
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| CN101440305A (en) * | 2007-11-22 | 2009-05-27 | 中国石油大学(北京) | Hydro-upgrading method for FCC gasoline |
| CN101591567A (en) * | 2008-05-29 | 2009-12-02 | 中国石油化工股份有限公司 | A kind of method that reduces olefin(e) centent in the secondary processing of gasoline |
| CN102285859A (en) * | 2010-06-18 | 2011-12-21 | 中国石油化工股份有限公司 | Selective hydrogenation process for C4 material flow with high concentration of butadiene |
| CN103100400A (en) * | 2011-11-09 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation method of hydrocracking catalyst |
-
2015
- 2015-05-25 CN CN201510270390.9A patent/CN105032474B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1352231A (en) * | 2000-11-08 | 2002-06-05 | 中国石油化工股份有限公司 | Hydrogenating and pour point depressing catalyst and its preparing method |
| CN1470614A (en) * | 2003-07-01 | 2004-01-28 | 中国石油天然气集团公司 | Catalyst for hydrogenation of olefin-containing naphtha and its preparing method |
| CN1590353A (en) * | 2003-08-26 | 2005-03-09 | 中国石化集团齐鲁石油化工公司 | Utilization method of butadiene extraction device residue |
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