CN102773106A - Catalyst for preparing low carbon olefin by synthetic gas as well as preparation method and application of catalyst - Google Patents
Catalyst for preparing low carbon olefin by synthetic gas as well as preparation method and application of catalyst Download PDFInfo
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- CN102773106A CN102773106A CN2012102574270A CN201210257427A CN102773106A CN 102773106 A CN102773106 A CN 102773106A CN 2012102574270 A CN2012102574270 A CN 2012102574270A CN 201210257427 A CN201210257427 A CN 201210257427A CN 102773106 A CN102773106 A CN 102773106A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention relates to a catalyst for directly preparing low carbon olefin by synthetic gas. The proportion (mole ratio) of the used raw materials comprising Fe, Mn and carbon source is (3-1):1: (2.5-10); the potassium soaking amount is based on the mole ratio of Fe to K being (80-20): 1; the catalyst is prepared by a hydrothermal in-situ synthesis method and a soaking method; and the performance indexes are as follows: CO conversion per pass is more than 95%, Olefin-to-polysilazane ratio (O/P) is more than 4.4, and content of C5<+> (middle C5)-C12 is 93%. The key point of the invention is to provide an innovative preparation method for the catalyst, namely the required active components are uniformly mixed with the used organic carbon source according to the proportion of the raw materials by the hydrothermal synthesis method, and the obtained mixture is reacted in a shorter time at a certain temperature so as to obtain catalyst powder.
Description
Technical field
The invention provides a kind of by synthesis gas (H
2And CO) catalyst of direct producing light olefins (ethene, propylene and butylene).Relate to a kind of catalyst and method for making and application that is used for the direct producing light olefins of synthesis gas specifically.
Background technology
Low-carbon alkene such as ethene, propylene is important basic Organic Chemicals; Along with the development of petrochemical industry, its demand is more and more big, is mainly derived from the catalytic pyrolysis by-product of naphtha or light diesel fuel at present; Along with the exhaustion day by day of petroleum resources, following energy resource structure certainly will shift.Compare with petroleum resources; Coal and natural gas resource are abundant relatively; With coal-based or natural gas base synthesis gas is raw material; Through the important channel that the synthetic direct producing light olefins production technology of Fischer-Tropsch has been opened up the synthetic basic chemical raw materials of non-oil resource, this process route is succinct, investment is low, has economic advantages.At present, catalyst is catalyst based with load Fe to be main, and through modifications such as auxiliary agent such as Mn, Zn, alkali (soil) metal, rare earth elements, carrier is generally selected porous material.
The silica gel that CN101940958A discloses a kind of acid solution surface modification with sugar is that carrier loaded Fe is catalyst based.Overcome the strong interaction between carrier and the active component, improved catalytic activity.88.2% after the modification, C are brought up in 21.8% before by the modification of CO conversion ratio
2 =-C
4 =Selectivity is brought up to more than 55.4% by 15.8%.The catalyst easy-formation, the preparation method is simple, and technology is ripe, be beneficial to suitability for industrialized production, but catalyst activity is on the low side, CH
4Selectivity is high.
CN1065026A discloses a kind of preparation of ethylene by use of synthetic gas method, and catalyst adopts chemical precipitation method and mechanical mixing preparation, adopts noble metal or rare metal; Kind of chemical element surplus niobium, gallium, praseodymium, scandium, indium, cerium, lanthanum, the ytterbium etc. ten for example; Ethylene selectivity is 65%-94%, but the CO conversion ratio is low, only about 10%, 12% and 15%; CO recycles the increase energy consumption, and the catalyst cost is high.
CN1428193A discloses a kind of nanometer Fe Preparation of catalysts method by preparation of low carbon olefines by synthetic gas.Adopt laser pyrolysis processes to combine the combination technique of solid phase reaction to prepare with Fe
3C is main Fe base nano-catalyst, and catalytic activity is higher, CO Zhuan Huashuai>96%, ethene and propylene content 82%-92% in the gas-phase product, CH
4Content is low, and no high-carbon hydrocarbon generates; Catalyst preparation process is loaded down with trivial details, and the catalyst cost is high.
CN1537674A discloses a kind of Fe/ activated-carbon catalyst preparation method and application by preparation of ethylene by use of synthetic gas, propylene and butylene.Adopt vacuum impregnation technology, Fe and auxiliary agent high degree of dispersion, and reduce preparation cost greatly, the CO conversion ratio>96%, gas-phase product CH compound selective>69.5%, the selectivity of low-carbon alkene in hydrocarbon>68%; The catalyst preparation process route is simple, but molysite that uses in the Preparation of Catalyst and manganese salt are more expensive, and indissolubles such as ferric oxalate and manganese acetate are separated, and uses ethanol to make corresponding cost of material and the running cost of having increased of solvent.
CN1083415A discloses a kind of, K molecular sieve supported with MgO alkaline earth oxide or silica-rich zeolite
+Perhaps Cs
+Addition agent modified Fe-Mn catalyst has good synthesizing low-carbon alkene performance, CO Zhuan Huashuai>90%, Xi Tingxuanzexing>66%.
Above-mentioned catalyst system and catalyzing is all being obtained progress preferably aspect the direct producing light olefins of synthesis gas; But still there is following problem: traditional Fischer-Tropsch synthetic poor selectivity; Can not get effective control, do not break through product A-S-F regularity of distribution restriction, added value of product is lower; CO
2, CH
4Selectivity higher, reduced the synthesis gas utilization ratio; Higher and poor repeatability of Preparation of Catalyst cost etc.The problem that catalyst need solve is: the secondary hydrogenation reaction of alkene is the control of olefine selective, and the control of products distribution.
Summary of the invention
One of the object of the invention is to overcome the prior art defective, and a kind of catalyst of preparation of low carbon olefines by synthetic gas is provided;
Two of the object of the invention is to overcome the prior art defective, and a kind of Preparation of catalysts method of preparation of low carbon olefines by synthetic gas is provided;
Three of the object of the invention is to overcome the prior art defective, and a kind of above-mentioned Application of Catalyst method is provided.
The object of the invention is realized according to following technical proposals:
A kind of catalyst that is used for the direct producing light olefins of synthesis gas, raw materials used proportioning (mol ratio) is Fe: Mn: carbon source=(3-1): 1: (2.5-10), the potassium pickup is pressed Fe/K mol ratio (80-20): 1; Adopt the hydro-thermal original position to synthesize with infusion process and process, its performance indications are: CO Dan Chengzhuanhuashuai>95%, ethylenic alkoxy rate (O/P)>4.4, C
5 +Middle C
5-C
12Han Liang>93%.
A kind of Preparation of catalysts method that is used for the direct producing light olefins of synthesis gas prepares through following steps:
(a) by Fe: Mn: carbon source=(3-1): 1: mol ratio (2.5-10) takes by weighing carbon source, ferric nitrate, manganese nitrate, is mixed with the homogeneous mixture solotion of 0.5-3mol/L;
(b) above-mentioned mixed solution is changed over to water heating kettle and places insulating box, rise to 150-200 ℃ with 2 ℃/min speed, constant temperature 2-8h;
(c) naturally after the cooling, filter, gains are dry in 80-120 ℃ of baking oven, powdered rubber A;
(d) the configuration solution of potassium carbonate as maceration extract, is impregnated into above-mentioned A with it, and 80-120 ℃ of drying gets powder B;
(e) gained B material is ground granulation to the 20-40 order, get catalyst;
Said carbon source is: a kind of or its combination in glucose, fructose, sucrose, the maltose etc.;
Above-mentioned potassium pickup is (80-20) according to the Fe/K mol ratio: 1.
Said Application of Catalyst is that the condition of fixed bed in-situ reducing is with its catalyst as preparation of low carbon olefines by synthetic gas: temperature 260-320 ℃, and pressure 0.1-0.5MPa, air speed 500-1500h
-1, reducing gases is formed H
2/ CO mol ratio is 1: 1-3: 1, and reduction 8-24h.
Described Application of Catalyst is that the condition of fixed bed catalyst is with its catalyst as preparation of low carbon olefines by synthetic gas: temperature 280-360 ℃, and pressure 0.5-2.5MPa, air speed 500-3000h
-1, unstripped gas is formed H
2/ CO is than 1: 1-3: 1.
Key of the present invention is the novelty of method for preparing catalyst, promptly adopts hydrothermal synthesis method that required active component is evenly mixed with used organic carbon source by proportioning raw materials, at a certain temperature, the short period internal reaction can obtain catalyst powder.
Advantage of the present invention is:
1. Preparation of Catalyst low in raw material cost of the present invention, be easy to get, preparation technology is simple, and the Preparation of Catalyst cost is low, is suitable for suitability for industrialized production.
2. the catalyst of the present invention's preparation adopts hydro-thermal method synthetic, and manufacturing cycle is short, uniform particles, good reproducibility.
3. catalyst of the present invention is used for synthesis gas and directly prepares low-carbon alkene reactivity height, Dan Chengzhuanhuashuai>95%, CH
4Selectivity<12%, CO
2Selectivity<16%, total olefin Shou Shuai>64g/ [Nm
3(CO+H
2)], and by-product light oil constituents, wherein C
5 +C in the component
5-C
12Chong Lianghanliang>93%.
The specific embodiment
Embodiment 1
Take by weighing Fe (NO
3)
39H
2O24.24g, 50wt%Mn (NO
3)
2Solution 7.16g, glucose 19.82g is mixed with homogeneous mixture solotion 100mL, changes in the water heating kettle; Place baking oven to rise to 170 ℃ with 2 ℃/min speed water heating kettle, constant temperature 4h after the cooling, filters naturally, after the 120C drying, grinds evenly; Take by weighing K
2CO
30.06g wiring solution-forming takes by weighing the 6.0g dried powder simultaneously, incipient impregnation is in joining K
2CO
3In the solution, 80 ℃ of dry 12h; Compressing tablet granulation 20-40 order.Catalyst reduction condition: H
2/ CO=2,0.1MPa, 280 ℃, air speed 500h
-1Reduction 12h; Activity rating condition: H
2/ CO=2,1.5MPa, 300C, air speed 500h
-1The result sees table 1.
Embodiment 2
Take by weighing Fe (NO
3)
39H
2O24.24g, 50wt%Mn (NO
3)
2Solution 7.16g, glucose 19.82g is mixed with mixed solution 100mL, changes in the water heating kettle; Place baking oven to rise to 180C with 2C/min speed water heating kettle, constant temperature 4h after the cooling, filters naturally, after the 120C drying, grinds evenly; Take by weighing K
2CO
30.12g wiring solution-forming takes by weighing the 6.0g dried powder simultaneously, incipient impregnation is in joining K
2CO
3In the solution, the dry 8h of 110C; Compressing tablet granulation 20-40 order.Catalyst reduction condition: H
2/ CO=2,0.1MPa, 300 ℃, air speed 1000h
-1Reduction 8h; Activity rating condition: H
2/ CO=2,1.5MPa, 320 ℃, air speed 500h
-1The result sees table 1.
Embodiment 3
Take by weighing Fe (NO
3)
39H
2O24.24g, 50wt%Mn (NO
3)
2Solution 10.74g, glucose 39.64g is mixed with mixed solution 100mL, changes in the water heating kettle; Place baking oven to rise to 180 ℃ with 2 ℃/min speed water heating kettle, constant temperature 4h after the cooling, filters naturally, after 120 ℃ of dryings, grinds evenly; Take by weighing K
2CO
30.06g wiring solution-forming takes by weighing the 6.0g dried powder simultaneously, incipient impregnation is in joining K
2CO
3In the solution, the dry 16h of 80C; Compressing tablet granulation 20-40 order.Catalyst reduction condition: H
2/ CO=2,0.1MPa, 280 ℃, air speed 500h
-1Reduction 12h; Activity rating condition: H
2/ CO=2,1.0MPa, 320C, air speed 1500h
-1The result sees table 1.
Embodiment 4
Take by weighing Fe (NO
3)
39H
2O24.24g, 50wt%Mn (NO
3)
2Solution 7.16g, sucrose 34.23g is mixed with homogeneous mixture solotion 100mL, changes in the water heating kettle; Place baking oven to rise to 190C with 2C/min speed water heating kettle, constant temperature 4h after the cooling, filters naturally, after the 120C drying, grinds evenly; Take by weighing K
2CO
30.06g wiring solution-forming takes by weighing the 6.0g dried powder simultaneously, incipient impregnation is in joining K
2CO
3In the solution, 110 ℃ of dry 8h; Compressing tablet granulation 20-40 order.Catalyst reduction condition: H
2/ CO=1,0.1MPa, 280C, air speed 500h
-1, reduction 8h; Activity rating condition: H
2/ CO=1,1.5MPa, 330C, air speed 500h
-1The result sees table 1.
Embodiment 5
Take by weighing Fe (NO
3)
39H
2O24.24g, 50wt%Mn (NO
3)
2Solution 7.16g, fructose 18.01g is mixed with homogeneous mixture solotion 100mL, changes in the water heating kettle; Place baking oven to rise to 180C with 2C/min speed water heating kettle, constant temperature 4h after the cooling, filters naturally, after the 120C drying, grinds evenly; Take by weighing K
2CO
30.12g wiring solution-forming takes by weighing the 6.0g dried powder simultaneously, incipient impregnation is in joining K
2CO
3In the solution, the dry 8h of 110C; Compressing tablet granulation 20-40 order.Catalyst reduction condition: H
2/ CO=1,0.1MPa, 280C, air speed 500h
-1, reduction 8h; Activity rating condition: H
2/ CO=1,1.5MPa, 330C, air speed 500h
-1The result sees table 1.
Embodiment 6
Take by weighing Fe (NO
3)
39H
2O24.24g, 50wt%Mn (NO
3)
2Solution 14.25g, maltose 36.03g is mixed with mixed solution 100mL, changes in the water heating kettle; Place baking oven to rise to 180C with 2C/min speed water heating kettle, constant temperature 4h after the cooling, filters naturally, after the 120C drying, grinds evenly; Take by weighing K
2CO
30.12g wiring solution-forming takes by weighing the 6.0g dried powder simultaneously, incipient impregnation is in joining K
2CO
3In the solution, the dry 8h of 110C; Compressing tablet granulation 20-40 order.Catalyst reduction condition: H
2/ CO=2,0.1MPa, 280C, air speed 500h
-1, reduction 8h; Activity rating condition: H
2/ CO=2,1.5MPa, 320C, air speed 800h
-1The result sees table 1.
The embodiment reaction result is seen table 1
Annotate: O/P is C
2-4 =/ C
2-4 0Content ratio.
Claims (6)
1. catalyst that is used for the direct producing light olefins of synthesis gas, raw materials used proportioning (mol ratio) is Fe: Mn: carbon source=(3-1): 1: (2.5-10), the potassium pickup is pressed Fe/K mol ratio (80-20): 1; Adopt the hydro-thermal original position to synthesize with infusion process and process, its performance indications are: CO Dan Chengzhuanhuashuai>95%, ethylenic alkoxy rate (O/P)>4.4, C
5 +Middle C
5-C
12Han Liang>93%.
2. Preparation of catalysts method that is used for the direct producing light olefins of synthesis gas prepares through following steps:
(a) by Fe: Mn: carbon source=(3-1): 1: mol ratio (2.5-10) takes by weighing carbon source, ferric nitrate, manganese nitrate, is mixed with the homogeneous mixture solotion of 0.5-3mol/L;
(b) change above-mentioned mixed solution over to water heating kettle, place insulating box, rise to 150-200 ℃ with 2C/min speed, constant temperature 2-8h;
(c) naturally after the cooling, filter, gains are dry in 80-120 ℃ of baking oven, powdered rubber A;
(d) configuration solution of potassium carbonate, and with it as maceration extract, be impregnated into above-mentioned A, 80-120 ℃ of drying, powder B;
(e) gained B material is ground granulation to the 20-40 order, get catalyst.
3. preparation method as claimed in claim 2 is characterized in that used carbon source is: a kind of or its combination in glucose, fructose, sucrose, the maltose etc.
4. preparation method as claimed in claim 2 is characterized in that the potassium pickup is (80-20) according to the Fe/K mol ratio: 1.
5. Application of Catalyst as claimed in claim 1 is characterized in that the condition of fixed bed in-situ reducing is with its catalyst as preparation of low carbon olefines by synthetic gas: temperature 260-320 ℃, and pressure 0.1-0.5MPa, air speed 500-1500h
-1, reducing gases is formed H
2/ CO mol ratio is 1: 1-3: 1, and reduction 8-24h.
6. Application of Catalyst as claimed in claim 1 is characterized in that the condition of fixed bed catalyst is with its catalyst as preparation of low carbon olefines by synthetic gas: temperature 280-360 ℃, and pressure 0.5-2.5MPa, air speed 500-3000h
-1, unstripped gas is formed H
2/ CO is than 1: 1-3: 1.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103212399A (en) * | 2013-04-19 | 2013-07-24 | 宁夏大学 | Preparation method and application for low carbon olefin zirconium-based catalyst through synthesis gas |
| CN105195205A (en) * | 2015-10-29 | 2015-12-30 | 江南大学 | Preparation and application of N-doped Fe-based catalyst for Fischer-Tropsch reaction |
| CN107827691A (en) * | 2017-11-06 | 2018-03-23 | 中石化炼化工程（集团）股份有限公司 | A kind of method of synthesis gas preparing low-carbon olefins |
| CN108620089A (en) * | 2018-05-30 | 2018-10-09 | 中国科学院广州能源研究所 | A kind of hydrogenation of carbon dioxide producing light olefins catalyst and the preparation method and application thereof |
| CN109912373A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | For preparation of low carbon olefines by synthetic gas catalyst and preparation method thereof |
| CN112206783A (en) * | 2020-10-19 | 2021-01-12 | 宁夏大学 | Preparation method and application of perovskite type oxygen carrier |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103212399A (en) * | 2013-04-19 | 2013-07-24 | 宁夏大学 | Preparation method and application for low carbon olefin zirconium-based catalyst through synthesis gas |
| CN105195205A (en) * | 2015-10-29 | 2015-12-30 | 江南大学 | Preparation and application of N-doped Fe-based catalyst for Fischer-Tropsch reaction |
| CN107827691A (en) * | 2017-11-06 | 2018-03-23 | 中石化炼化工程（集团）股份有限公司 | A kind of method of synthesis gas preparing low-carbon olefins |
| CN109912373A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | For preparation of low carbon olefines by synthetic gas catalyst and preparation method thereof |
| CN109912373B (en) * | 2017-12-13 | 2022-03-08 | 中国石油化工股份有限公司 | Catalyst for preparing low-carbon olefin from synthesis gas and preparation method thereof |
| CN108620089A (en) * | 2018-05-30 | 2018-10-09 | 中国科学院广州能源研究所 | A kind of hydrogenation of carbon dioxide producing light olefins catalyst and the preparation method and application thereof |
| CN108620089B (en) * | 2018-05-30 | 2021-01-29 | 中国科学院广州能源研究所 | Catalyst for preparing low-carbon olefin by carbon dioxide hydrogenation and preparation method and application thereof |
| CN112206783A (en) * | 2020-10-19 | 2021-01-12 | 宁夏大学 | Preparation method and application of perovskite type oxygen carrier |
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Application publication date: 20121114 |