CN102794167A - Catalyst for preparing isobutene by isobutane dehydrogenation and preparation method for catalyst - Google Patents
Catalyst for preparing isobutene by isobutane dehydrogenation and preparation method for catalyst Download PDFInfo
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- CN102794167A CN102794167A CN2012101972410A CN201210197241A CN102794167A CN 102794167 A CN102794167 A CN 102794167A CN 2012101972410 A CN2012101972410 A CN 2012101972410A CN 201210197241 A CN201210197241 A CN 201210197241A CN 102794167 A CN102794167 A CN 102794167A
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- isobutene
- dehydrogenation
- isobutane
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- 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 provides a catalyst for preparing isobutene by isobutane dehydrogenation and a preparation method for the catalyst. The catalyst comprises the following components in percentage by mass: 60 to 90 percent of Cr2O3, 3 to 12 percent of CaO, 0.5 to 3.0 percent of K2O and 5 to 36.5 percent of Al2O3. The preparation method comprises the following steps of: adding Cr2O3, CaO, K2O and Al2O3 into an aqueous solution of diluted nitric acid in an abundance ratio, baking, introducing nitrogen, roasting, decomposing nitrate and performing solid ion exchange, and thus obtaining the Cr2O3-CaO-K2O-Al2O3 catalyst. The invention has the advantages that the preparation flow of the catalyst is simple, and preparation and use of the catalyst and the waste catalyst do not pollute the environment; the catalyst for preparing the isobutene by the isobutane dehydrogenation has activity and stability, and particularly has excellent isobutene selectivity; and the conversion per pass of isobutane is over 50 percent, and the selectivity of the isobutene serving as a target product is over 98 percent.
Description
Technical field
The present invention relates to Preparation of catalysts, is that dehydrogenation of isobutane prepares the used Catalysts and its preparation method of isobutene specifically.
Background technology
Isobutene is a kind of very important organic chemical industry's intermediate; Be mainly used in preparation methyl tertiary butyl ether(MTBE) (MTBE; High-octane rating clean gasoline blend component), butyl rubber, polyisobutene, methacrylate, tertiary butyl phenol, tert-butylamine, 1, various Organic Ingredients and fine chemicals such as 4-butanediol, ABS resin.
Along with continually developing of isobutene downstream product and derivative thereof, the demand of isobutene enlarges day by day, and conventional steam cracking process is because the restriction of himself production technology is restricted the isobutene raising the output.In addition, along with the development of gas industry, the liquefied petroleum gas of petroleum refining industry progressively dwindles as the market of domestic fuel, and the chemical utilization technology of exploitation liquefied petroleum gas is that petroleum refining industry is increased the benefit and one of key of the level of resources utilization.Contain a large amount of iso-butane resources in the liquefied petroleum gas, therefore developing dehydrogenation of isobutane prepares isobutene, is to expand isobutene raw material sources and an important channel of improving the petroleum refining industry benefit.
The existing in the world at present industrialized dehydrogenation of isobutane of several covers prepares the isobutene technology, comprises FBD-4 and the Linde technology of German Linde company of star technology and Italian Snamprogetti SPA company of catofin technology, the Phillips company of oleflex technology, the ABB Lummus of American UOP company.The catalyst that dehydrogenation of isobutane prepares isobutene mainly is divided into two big types, chromium-based catalysts and platinum family noble metal catalyst.The Catalysts and its preparation method of carried noble metal platinum on alumina support is disclosed like USP4506032, USP4595673 etc.; Like Hakuli etc. on 11%CrOx/SiO2 (in the mass fraction of Cr) catalyst; Obtained 18% isobutene yield in the time of 540 ℃, but the selectivity of isobutene lower (72%), and have serious carbon distribution phenomenon; Cause catalysqt deactivation (A. Hakuli; Et al. J. Catal., 1999,184:349-356).These traditional dehydrogenation of isobutane prepare the method for isobutene, and are high because of reaction temperature, reaction velocity is low and catalyst surface is prone to problem such as carbon distribution and causes its target product selectivity low, and catalyst is prone to inactivation.
Low-carbon alkanes oxidative dehydrogenation is a kind of exothermic reaction, can under lower temperature, carry out, and again because the introducing of oxygen can be eliminated the catalyst surface carbon distribution, thereby the isobutene for oxo-dehydrogenation producing of isobutylene method is received publicity.As all disclosing the catalyst and the process of isobutene for oxo-dehydrogenation producing of isobutylene in the patents such as CN101138738B, CN1044787C, CN101439292A, CN101618319A.Yet in the presence of oxygen, the deep oxidation reaction be prone to take place in the target product alkene of isobutene for oxo-dehydrogenation and raw material iso-butane, causes problems such as the selectivity of raw material iso-butane and target product alkene is low.Therefore, it is significant that the dehydrogenation of isobutane of developing a kind of high selectivity and high conversion prepares the catalyst of isobutene.
Summary of the invention
The objective of the invention is to overcome the weak point that exists in the prior art, and provide the dehydrogenation of isobutane of a kind of high activity, high selectivity to prepare the used Catalysts and its preparation method of isobutene.
The object of the invention can realize through following measure: dehydrogenation of isobutane prepares the used catalyst of isobutene, this catalyst Cr
2O
3Content be that the 60-90% of catalyst quality mark, the content of CaO are 3-12%, the K of catalyst quality mark
2The content of O is 0.5-3.0%, the Al of catalyst quality mark
2O
3Content be the 5-36.5% of catalyst quality mark.
Described active component chrome green is to introduce with the chrome green powder type; Calcium oxide and potassium oxide be to introduce with the form of nitric acid calcium salt, potassium salt; Alundum (Al is to introduce with the activated alumina form of powder.
Dehydrogenation of isobutane prepares the used Preparation of catalysts method of isobutene, and this method is according to Cr
2O
3, CaO, K
2O, Al
2O
3Content ratio, take by weighing chrome green powder, active oxidation aluminium powder, nitric acid calcium salt, potassium nitrate, join mass concentration and be in 10% the diluted nitric acid aqueous solution; Mix, knead evenly back extrusion; 120 ℃ of baking ovens baking 24 hours, logical nitrogen in resistance furnace, 540 ℃ of roastings 4 hours; Nitrate is decomposed and the exchange of realization solid ionic, obtain Cr
2O
3– CaO-K
2O-Al
2O
3Dehydrogenation of isobutane prepares isobutene catalyst.
The present invention prepares in the isobutene reaction at dehydrogenation of isobutane; The trivalent chromium species have excellent dehydrogenation activity; And the acid intensity of catalyst and distribution are to influence optionally principal element; Therefore to improve dehydrogenation of isobutane activity of such catalysts and selectivity, the trivalent chromium species on the just necessary rugged catalyst, the acidity of regulating catalyst distributes and acid strength; Trivalent chromium does not have harm to environment simultaneously, and the valence state of rugged catalyst chromium species not only can make catalyst have high dehydrogenation of isobutane activity and activity stability, and has eliminated the pollution of Cr VI element to environment.The invention reside in provides a kind of solid ionic exchange preparation solid Cr
2O
3– CaO-K
2O-Al
2O
3Dehydrogenation of isobutane prepares isobutene catalyst and method thereof, Cr
2O
3Be the activity of such catalysts constituent element; K
2O is an electronics property auxiliary agent, modulation active component Cr
2O
3The electronics form; CaO and Al
2O
3Interact, modulation is as binding agent Al
2O
3Acid intensity and distribution, thereby realize that high activity and activity stability, environmental friendliness dehydrogenation of isobutane prepare synthesizing of isobutene catalyst.
The present invention compared with prior art has following advantage:
1, the Preparation of Catalyst flow process is simple, Preparation of Catalyst, uses and discarded catalyst can not cause environmental pollution;
2, catalyst has high dehydrogenation of isobutane and prepares isobutene activity, activity stability, especially has excellent selective isobutene; Under certain reaction condition, can realize that the iso-butane conversion per pass more than 50%, reaches more than 98% the target product selective isobutene.
The specific embodiment
Following embodiment describes in further detail of the present invention, but the present invention does not receive the restriction of these embodiment.
Embodiment 1
Take by weighing 60g chrome green powder (Tianjin Chemical Plant production) respectively, Cr
2O
3Content be 60% of catalyst quality mark; 36.5g active alchlor (production of Sinopec Chang Ling catalyst plant), Al
2O
3Content be 36.5% of catalyst quality mark; 8.78g calcium nitrate (Beijing chemical reagents corporation), the content of CaO is 3.0% of catalyst quality mark; With 0.54g potassium nitrate (Beijing chemical reagents corporation), K
2The content of O is 0.5% of catalyst quality mark, is 10% diluted nitric acid aqueous solution 10g grinding and drip mass concentration, stir, kneading, and be extruded moulding on 0.5 millimeter the banded extruder at the plate hole diameter then.With the mixture bar of extruded moulding 120 ℃ of bakings 24 hours, again with the oxidation aluminum strip of oven dry 540 ℃ of logical nitrogen roastings 4 hours down, obtain the solid that 100g realizes the solid ionic exchange, it consists of Cr
2O
3: CaO:K
2O:Al
2O
3Mass ratio be 60:3:0.5:36.5, be cut into 10-20 purpose particle, be called catalyst A, subsequent use.Each material content of following examples by that analogy.
Embodiment 2
Take by weighing 70g chrome green powder (Tianjin Chemical Plant production) respectively; The active alchlor (production of Sinopec Chang Ling catalyst plant) of 23g; 17.56g calcium nitrate (Beijing chemical reagents corporation) and 1.07g potassium nitrate (Beijing chemical reagents corporation); Grinding and drip mass concentration is that 10% diluted nitric acid aqueous solution 15g stirs, kneading, is extruded moulding on 0.5 millimeter the banded extruder at the plate hole diameter then.With the mixture bar of extruded moulding 120 ℃ of bakings 24 hours, again with the oxidation aluminum strip of oven dry 540 ℃ of logical nitrogen roastings 4 hours down, obtain the solid that 100g realizes the solid ionic exchange, it consists of Cr
2O
3: CaO:K
2O:Al
2O
3Mass ratio be 70:6:1.0:23, be cut into 10-20 purpose particle, be called catalyst B, subsequent use.
Embodiment 3
Take by weighing 70g chrome green powder (Tianjin Chemical Plant production), the active alchlor (production of Sinopec Chang Ling catalyst plant) of 16g, 35.11g calcium nitrate (Beijing chemical reagents corporation) and 2.15g potassium nitrate (Beijing chemical reagents corporation) respectively; Grinding and drip mass concentration is that 10% diluted nitric acid aqueous solution 15g stirs, kneading, is extruded moulding on 0.5 millimeter the banded extruder at the plate hole diameter then.With the mixture bar of extruded moulding 120 ℃ of bakings 24 hours, again with the oxidation aluminum strip of oven dry 540 ℃ of logical nitrogen roastings 4 hours down, obtain the solid that 100g realizes the solid ionic exchange, it consists of Cr
2O
3: CaO:K
2O:Al
2O
3Mass ratio be 70:12:2.0:16, be cut into 10-20 purpose particle, be called catalyst C, subsequent use.
Embodiment 4
Take by weighing 80g chrome green powder (Tianjin Chemical Plant production), the active alchlor (production of Sinopec Chang Ling catalyst plant) of 11g, 17.56g calcium nitrate (Beijing chemical reagents corporation) and 3.22g potassium nitrate (Beijing chemical reagents corporation) respectively; Grinding and drip mass concentration is that 10% diluted nitric acid aqueous solution 15g stirs, kneading, is extruded moulding on 0.5 millimeter the banded extruder at the plate hole diameter then.With the mixture bar of extruded moulding 120 ℃ of bakings 24 hours, again with the oxidation aluminum strip of oven dry 540 ℃ of logical nitrogen roastings 4 hours down, obtain the solid that 100g realizes the solid ionic exchange, it consists of Cr
2O
3: CaO:K
2O:Al
2O
3Mass ratio be 80:6:3.0:11, be cut into 10-20 purpose particle, be called catalyst D, subsequent use.
Embodiment 5
Take by weighing 90g chrome green powder (Tianjin Chemical Plant production), the active alchlor (production of Sinopec Chang Ling catalyst plant) of 6.5g, 8.78g calcium nitrate (Beijing chemical reagents corporation) and 0.5g potassium nitrate (Beijing chemical reagents corporation) respectively; Grinding and drip mass concentration is that 10% diluted nitric acid aqueous solution 15g stirs, kneading, is extruded moulding on 0.5 millimeter the banded extruder at the plate hole diameter then.With the mixture bar of extruded moulding 120 ℃ of bakings 24 hours, again with the oxidation aluminum strip of oven dry 540 ℃ of logical nitrogen roastings 4 hours down, obtain the solid that 100g realizes the solid ionic exchange, it consists of Cr
2O
3: CaO:K
2O:Al
2O
3Mass ratio be 90:3:0.5:6.5, be cut into 10-20 purpose particle, be called catalyst E, subsequent use.
The test of embodiment 6 catalyst performance evaluation
Raw material iso-butane (Shijiazhuang Oil Refinery) delivers into fixed bed reactors (granularity of catalyst is the 10-20 order for the stainless steel reactor of internal diameter 12mm, constant temperature head of district 15cm, and the catalyst bed layer thickness is 9-10cm) through feed pump.Product is after counterbalance valve decompression, and pressure is reduced to normal pressure, flows into the low pressure product separator, collects the back product chromatography analysis of supplying gas.The raw material inlet amount is controlled by feed pump.Adding electrothermal stove provides reaction needed temperature.
Reaction temperature is that 550 ℃-650 ℃, reaction pressure are that 0.1MPa-1.0MPa, reaction mass air speed are 0.6-2.0 h
-1Scope in, reaction result is seen table 1.
Table 1 dehydrogenation of isobutane prepares isobutene catalyst performance evaluation result
| The catalyst title | The iso-butane conversion ratio, l% | Selective isobutene, % |
| A | 51.5 | 98.1 |
| B | 53.4 | 98.5 |
| C | 56.4 | 99.2 |
| D | 52.3 | 97.8 |
| E | 54.5 | 98.4 |
Claims (3)
1. dehydrogenation of isobutane prepares the used catalyst of isobutene, it is characterized in that: this catalyst Cr
2O
3Content be that the 60-90% of catalyst quality mark, the content of CaO are 3-12%, the K of catalyst quality mark
2The content of O is 0.5-3.0%, the Al of catalyst quality mark
2O
3Content be the 5-36.5% of catalyst quality mark.
2. dehydrogenation of isobutane according to claim 1 prepares the used catalyst of isobutene, it is characterized in that: the active component chrome green is to introduce with the chrome green powder type; Calcium oxide and potassium oxide be to introduce with the form of nitric acid calcium salt, potassium salt; Alundum (Al is to introduce with the activated alumina form of powder.
3. prepare the used Preparation of catalysts method of isobutene by the described dehydrogenation of isobutane of claim 1, it is characterized in that: this method is according to Cr
2O
3, CaO, K
2O, Al
2O
3Content ratio, take by weighing chrome green powder, active oxidation aluminium powder, nitric acid calcium salt, potassium nitrate, join mass concentration and be in 10% the diluted nitric acid aqueous solution; Mix, knead evenly back extrusion; 120 ℃ of baking ovens baking 24 hours, logical nitrogen in resistance furnace, 540 ℃ of roastings 4 hours; Nitrate is decomposed and the exchange of realization solid ionic, obtain Cr
2O
3– CaO-K
2O-Al
2O
3Dehydrogenation of isobutane prepares isobutene catalyst.
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|---|---|---|---|
| CN2012101972410A CN102794167A (en) | 2012-06-15 | 2012-06-15 | Catalyst for preparing isobutene by isobutane dehydrogenation and preparation method for catalyst |
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|---|---|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044180A (en) * | 2012-12-28 | 2013-04-17 | 北京石油化工学院 | Method for preparing isobutylene by dehydrogenizing iso-butane |
| CN104043443A (en) * | 2014-06-13 | 2014-09-17 | 烟台大学 | High-intensity low-carbon alkane dehydrogenation catalyst and preparation method thereof |
| CN104128175A (en) * | 2014-07-07 | 2014-11-05 | 烟台大学 | Light alkane dehydrogenation catalyst with good hydrothermal stability and preparation method thereof |
| CN104437515A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Low-carbon alkane dehydrogenation catalyst and use method thereof |
| CN106944079A (en) * | 2016-01-07 | 2017-07-14 | 中国石油化工股份有限公司 | A kind of preparation method of iso-butane preparing isobutene catalyst |
| CN107715862A (en) * | 2017-09-30 | 2018-02-23 | 大连理工大学 | A kind of anti-carbon chromium base catalyst for preparing propylene with propane dehydrogenation, preparation method and application |
| CN115779885A (en) * | 2021-09-10 | 2023-03-14 | 中国石油化工股份有限公司 | Light hydrocarbon dehydrogenation catalyst and preparation method and application thereof |
| WO2024133034A1 (en) | 2022-12-22 | 2024-06-27 | Sabic Global Technologies B.V. | Chromium oxide containing catalysts for paraffin dehydrogenation and methods of making and using thereof |
| WO2024133032A1 (en) | 2022-12-22 | 2024-06-27 | Sabic Global Technologies B.V. | Catalyst for paraffin dehydrogenation |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044180A (en) * | 2012-12-28 | 2013-04-17 | 北京石油化工学院 | Method for preparing isobutylene by dehydrogenizing iso-butane |
| CN104437515A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Low-carbon alkane dehydrogenation catalyst and use method thereof |
| CN104043443A (en) * | 2014-06-13 | 2014-09-17 | 烟台大学 | High-intensity low-carbon alkane dehydrogenation catalyst and preparation method thereof |
| CN104043443B (en) * | 2014-06-13 | 2016-06-08 | 烟台大学 | A kind of high strength low-carbon alkane dehydrogenating catalyst and its preparation method |
| CN104128175A (en) * | 2014-07-07 | 2014-11-05 | 烟台大学 | Light alkane dehydrogenation catalyst with good hydrothermal stability and preparation method thereof |
| CN106944079A (en) * | 2016-01-07 | 2017-07-14 | 中国石油化工股份有限公司 | A kind of preparation method of iso-butane preparing isobutene catalyst |
| CN106944079B (en) * | 2016-01-07 | 2019-06-11 | 中国石油化工股份有限公司 | A kind of preparation method of iso-butane preparing isobutene catalyst |
| CN107715862A (en) * | 2017-09-30 | 2018-02-23 | 大连理工大学 | A kind of anti-carbon chromium base catalyst for preparing propylene with propane dehydrogenation, preparation method and application |
| CN115779885A (en) * | 2021-09-10 | 2023-03-14 | 中国石油化工股份有限公司 | Light hydrocarbon dehydrogenation catalyst and preparation method and application thereof |
| CN115779885B (en) * | 2021-09-10 | 2024-05-03 | 中国石油化工股份有限公司 | Light hydrocarbon dehydrogenation catalyst and preparation method and application thereof |
| WO2024133034A1 (en) | 2022-12-22 | 2024-06-27 | Sabic Global Technologies B.V. | Chromium oxide containing catalysts for paraffin dehydrogenation and methods of making and using thereof |
| WO2024133032A1 (en) | 2022-12-22 | 2024-06-27 | Sabic Global Technologies B.V. | Catalyst for paraffin dehydrogenation |
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