CN102463132B - Method for preparing C5 hydrocarbon aromatization catalysts - Google Patents
Method for preparing C5 hydrocarbon aromatization catalysts Download PDFInfo
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- CN102463132B CN102463132B CN201010552824.1A CN201010552824A CN102463132B CN 102463132 B CN102463132 B CN 102463132B CN 201010552824 A CN201010552824 A CN 201010552824A CN 102463132 B CN102463132 B CN 102463132B
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Abstract
The invention relates to a method for preparing C5 hydrocarbon aromatization catalysts, which mainly aims at solving the problem of poor stability of the aromatization catalysts in the prior art. The method adopts the technical scheme that the method comprises the following steps that: a) ZSM-5 molecular sieves or compound materials after the ZSM-5 molecular sieves are formed with bonding agents are subjected to hydro-thermal treatment for 0.1 to 40 hours in alkali solution with the concentration being 0.01 to 1.0M under the temperature condition being 10 to 100 DEG C to obtain first precursors; b) the first precursors are washed, ammonia exchange and drying are carried out, then, at least one kind of elements selected from VIIIA, IIB and IIIB groups is loaded by an immersion method, and the loading quantity is 0.1 to 10 weight percent. The problem is perfectly solved, and the method can be used for industrial production of preparing aromatic hydrocarbons through C5 hydrocarbon aromatization.
Description
Technical field
The present invention relates to a kind of preparation method of C5 hydrocarbon aromatization catalyst.
Background technology
Aromatic hydrocarbons is widely used in synthetic fibers, synthetic resin, synthetic rubber and various fine chemicals, is indispensable basic organic chemical industry raw material, and non-benzene aromatic hydrocarbons is still produced the important mediation component of high-knock rating gasoline in addition.In recent years, aromatic hydrocarbons downstream product development rapidly, causes the demand sustainable growth of domestic and international market to aromatic hydrocarbons, wherein China to aromatic hydrocarbons year the growth rate of demand more than 10%.
C5 alkane and the hydrocarbon mixture that contains C5 alkane are the byproducts of petrochemical industry and oil refining industry, originate from ethylene project, oil plant and natural gas purification process.Estimate to the year two thousand twenty, carbon five total resources of China will reach 1,000 ten thousand tons of left and right.Because the boiling point of C5 hydro carbons is lower, 36 ℃ of left and right, under normal temperature, be the liquid of highly volatile, neither gasoline component, neither liquefied petroleum gas component, very major part is all used as cheap fuel.These C5 hydro carbons are converted into aromatic hydrocarbons by technology of aromatization, not only can be aromatic hydrocarbons production and open up new raw material source, and can optimize and utilize lighter hydrocarbons resource, improve petroleum chemical enterprise's economic benefit.
Researcher is very active in the research in light-hydrocarbon aromatized field both at home and abroad at present.
Patent CN1341699A discloses a kind of take HZSM-5 zeolite and aluminium oxide as carrier, take Zn and Ni as the aromatization of low carbon hydrocarbon method for preparing catalyst of active metal component, wherein in metal impregnation liquid, has added a small amount of competition buffer and surfactant.At 540～560 ℃, 0.5～1MPa, volume space velocity is 0.5～2h
-1under condition, for mixing carbon four aromatizations, catalyst single pass life reaches 120h.
Patent CN1990104A discloses a kind of method for preparing catalyst that improves hydrogen type molecular sieve aromatization stability by alkali treatment modifying, for the treatment of the liquefied gas that is rich in alkene, the alkene in raw material can be converted into the gasoline that is rich in non-benzene aromatic hydrocarbons.At 250～450 ℃, pressure 0.5～50atm, weight space velocity 0.1～10h
-1reaction condition under, catalyst single pass life reaches 60h.
Patent CN101530813A discloses a kind of molecular sieve catalyst preparation method for carbon 4 liquid gas aromatization reaction, and adopting rare earth-ZSM-5/ZSM-11 cocrystallization molecular sieve is parent, through making catalyst after alkali treatment-steam treatment-zinc supported.At 470～520 ℃, pressure 0.3～0.9MPa, weight space velocity 0.5～1.5h
-1reaction condition under, catalyst single pass life 30h, aromatics yield is 62wt%.
Patent CN1586721A discloses a kind of molecular sieve catalyst preparation method for carbon four liquefied petroleum gas aromatisation, and the silica-rich zeolite that employing grain size is 10～500nm, carries out steam treatment and sour reaming modification makes catalyst, does not add metal component.At 400 ℃, pressure 3MPa, weight space velocity 0.8h
-1reaction condition under, the single pass life of catalyst can reach 10 days, aromatics yield is 49wt%.
Patent CN1232071A discloses one and has been made up of Zn, rare earth, ZSM-5 and aluminium oxide, and has carried out the aromatized catalyst preparation method of steam treatment modification, and wherein Zn species are by [Zn (NH
3)
4]
2+form be introduced into molecular sieve catalyst.This catalyst is at 520～550 ℃, mass space velocity 0.6～1.5h
-1reaction condition under carry out aromatization to mixing carbon four, it is 300～450h that aromatics yield is greater than 40% one way duration of runs.
Patent CN1340601A discloses one and has been made up of ZnO, ZSM-5 molecular sieve, aluminium oxide and VA or group vib oxide, and has carried out the aromatized catalyst preparation method of steam treatment modification, for the aromatization of n-hexane and mixing carbon four.This catalyst is at 450～600 ℃, pressure 0.1～1.0MPa, mass space velocity 0.2～12h
-1reaction condition under carry out aromatization to mixing carbon four, it is 470h that aromatics yield is greater than 41% one way duration of runs.
In above-mentioned technology, the single pass life of catalyst, all in 500h, shows that the reaction stability of catalyst is undesirable, and this causes reactor in course of reaction to switch regeneration frequently.Patent CN101580737A discloses a kind of molecular sieve catalyst preparation method for direct steaming gasoline and liquefied gas milling aromatization reaction, adopting rare earth-ZSM-5/ZSM-11 cocrystallization molecular sieve is parent, through making catalyst after alkali treatment-steam treatment.At 340～420 ℃, pressure 0.3MPa, weight space velocity 0.3h
-1reaction condition under, the single pass life of catalyst is 43 days, but aromatics yield is lower, is only 25wt%.
The object of this invention is to provide a kind of method for preparing catalyst of C5 aromatization of hydrocarbons, the catalyst of preparing by the method can obtain good reaction stability under the prerequisite that keeps higher aromatization activity.
Summary of the invention
Technical problem to be solved by this invention is the bad problem of aromatized catalyst reaction stability in prior art, and a kind of preparation method of new C5 hydrocarbon aromatization catalyst is provided.The catalyst of preparing by the method has advantages of and can under the prerequisite that keeps certain aromatization activity, show good reaction stability for C5 aromatization of hydrocarbons.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of preparation method of C5 hydrocarbon aromatization catalyst, comprises the following steps:
A) in the aqueous slkali that is 0.01～1.0M by the composite after ZSM-5 molecular sieve or ZSM-5 molecular sieve and binding agent moulding in concentration, in the Water Under heat treatment 0.1～40h of 10～100 ℃ of temperature, obtain precursor I.
B) by precursor I washing, ammonia exchange, dry, be selected from least one element in VIIIA, IIB and IIIB family by infusion process load afterwards, load capacity is 0.1～10wt%.
In technique scheme, the aqueous slkali adopting is at least one in NaOH, KOH and ammonia spirit; The alkaline concentration preferable range adopting is 0.1～0.6M; The treatment temperature preferable range adopting is 20～80 ℃; The processing time preferable range adopting is 0.5～30h; The metal species of institute's load comprise at least one element in VIIIA, IIB or IIIB family, and preferred negative carrying capacity is 0.1～5wt%; Handled raw material is C5 hydro carbons or the compound that contains C5 hydro carbons.
The method adopts the means of alkali treatment modifying by mesoporous introducing ZSM-5 molecular sieve, improve the mass transfer diffusivity of poromerics, and introduce one or more metal species and adjust sour density and the distribution of acids type on molecular sieve, improve aromatization activity, suppress the carbon distribution speed on catalyst, and then realize the more excellent reaction stability of acquisition in guaranteeing C5 aromatizing reaction of hydrocarbons activity.In the time that the mixed C 5 that is rich in alkene is made raw material, catalyst single pass life reaches 700h, aromatics yield 49wt%; In the time that the mixed C 5 that is rich in alkane is made raw material, catalyst single pass life reaches 1000h, and aromatics yield 38wt% has obtained good technique effect.
The included catalyst preparation process of the present invention is simple to operate, and required condition easily obtains and controls, and can alleviate reactor in existing commercial fixed bed device and switch and catalyst regeneration problem frequently.
Below by embodiment, the present invention is further elaborated.
The specific embodiment
[comparative example 1]
To remove the NaZSM-5 molecular sieve of template and boehmite, field mountain valley with clumps of trees and bamboo powder according to weight ratio ZSM-5: Al
2o
3: mountain valley with clumps of trees and bamboo powder=1, field: mix at 0.3: 0.1.In mixture, add appropriate salpeter solution, pinch even and extruded moulding, in 120 ℃ of dry 10h, 550 ℃ of roasting 3h, pelletizing.Molecular sieve after moulding, 80 ℃ of exchanges of the ammonium nitrate solution with 0.8mol/L 3 times, is washed 2 times, and 120 ℃ dry, and 550 ℃ of roasting 4h, obtain hydrogen type molecular sieve catalyst and be designated as A.
[comparative example 2]
Molecular sieve and forming process thereof are identical with comparative example 1.Molecular sieve after moulding, 80 ℃ of exchanges of the ammonium nitrate solution with 0.8mol/L 3 times, is washed 2 times, and 120 ℃ dry, obtains ammonia type molecular sieve used.By the molecular sieve carried Ga metal of incipient impregnation normal direction ammonia type species, load capacity is 3wt%, leaves standstill afterwards 4h, 120 ℃ of dry 10h, and 550 ℃ of roasting 4h, make catalyst, are designated as catalyst B.
[embodiment 1]
Molecular sieve and forming process thereof are identical with comparative example 1.ZSM-5 molecular sieve 20g after moulding is placed in to the NaOH solution of 200ml, 0.2M, 80 ℃ of waters bath with thermostatic control are also stirred 2h, and cool to room temperature filters, washs to neutral.Afterwards resulting materials is exchanged 3 times at 80 ℃ of ammonium nitrate solutions with 0.8mol/L, wash 2 times, 120 ℃ of dry 10h, obtain ammonia type molecular sieve.By the molecular sieve carried Ga metal of incipient impregnation normal direction ammonia type species, load capacity is 3wt%, leaves standstill afterwards 4h, 120 ℃ of dry 10h, and 550 ℃ of roasting 4h, make catalyst, are designated as catalyst C.
[embodiment 2]
Molecular sieve and forming process thereof are identical with comparative example 1.Molecular sieve 20g after moulding is placed in to the NaOH solution of 200ml, 0.4M, 90 ℃ of waters bath with thermostatic control are also stirred 1h, and cool to room temperature filters, washs to neutral.Afterwards resulting materials is exchanged 3 times at 80 ℃ of ammonium nitrate solutions with 0.8mol/L, wash 2 times, 120 ℃ of dry 10h, obtain ammonia type molecular sieve.By the molecular sieve carried Ga of incipient impregnation normal direction ammonia type and Ni metal species, load capacity is respectively 2wt% and 0.8wt%, leaves standstill afterwards 4h, 120 ℃ of dry 10h, and 550 ℃ of roasting 4h, make catalyst, are designated as catalyst D.
[embodiment 3]
Molecular sieve and forming process thereof are identical with comparative example 1.Molecular sieve 20g after moulding is placed in to the NaOH solution of 200ml, 0.2M, 50 ℃ of waters bath with thermostatic control are also stirred 6h, and cool to room temperature filters, washs to neutral.Afterwards resulting materials is exchanged 3 times at 80 ℃ of ammonium nitrate solutions with 0.8mol/L, wash 2 times, 120 ℃ of dry 10h, obtain ammonia type molecular sieve.By the molecular sieve carried Ni metal of incipient impregnation normal direction ammonia type species, load capacity is 3wt%, leaves standstill afterwards 4h, 120 ℃ of dry 10h, and 550 ℃ of roasting 4h, make catalyst, are designated as catalyst E.
[embodiment 4]
Molecular sieve and forming process thereof are identical with comparative example 1.The NaOH solution that molecular sieve 20g after moulding is placed in to 200ml, 0.8M, stirs 30h under room temperature, and cool to room temperature filters, washs to neutral.Afterwards resulting materials is exchanged 3 times at 80 ℃ of ammonium nitrate solutions with 0.8mol/L, wash 2 times, 120 ℃ of dry 10h, obtain ammonia type molecular sieve.By the molecular sieve carried Co metal of incipient impregnation normal direction ammonia type species, load capacity is 2wt%, leaves standstill afterwards 4h, 120 ℃ of dry 10h, and 550 ℃ of roasting 4h, make catalyst, are designated as catalyst F.
[embodiment 5]
Molecular sieve and forming process thereof are identical with comparative example 1.Molecular sieve 20g after moulding is placed in to the NaOH solution of 200ml, 0.4M, 50 ℃ of waters bath with thermostatic control are also stirred 6h, and cool to room temperature filters, washs to neutral.Afterwards resulting materials is exchanged 3 times at 80 ℃ of ammonium nitrate solutions with 0.8mol/L, wash 2 times, 120 ℃ of dry 10h, obtain ammonia type molecular sieve.By the molecular sieve carried Ga of incipient impregnation normal direction ammonia type and Fe metal species, load capacity is respectively 2wt% and 0.8wt%, leaves standstill afterwards 4h, 120 ℃ of dry 10h, and 550 ℃ of roasting 4h, make catalyst, are designated as catalyst G.
[embodiment 6]
Molecular sieve and forming process thereof are identical with comparative example 1.Molecular sieve 20g after moulding is placed in to the NaOH solution of 200ml, 0.3M, 70 ℃ of waters bath with thermostatic control are also stirred 5h, and cool to room temperature filters, washs to neutral.Afterwards resulting materials is exchanged 3 times at 80 ℃ of ammonium nitrate solutions with 0.8mol/L, wash 2 times, 120 ℃ of dry 10h, obtain ammonia type molecular sieve.By the molecular sieve carried Ni of incipient impregnation normal direction ammonia type, Zn and Fe metal species, load capacity is 1.0wt%, leaves standstill afterwards 4h, 120 ℃ of dry 10h, and 550 ℃ of roasting 4h, make catalyst, are designated as catalyst H.
[embodiment 7]
Molecular sieve and forming process thereof are identical with comparative example 1.Molecular sieve 20g after moulding is placed in to the NaOH solution of 200ml, 0.2M, 70 ℃ of waters bath with thermostatic control are also stirred 5h, and cool to room temperature filters, washs to neutral.Afterwards resulting materials is exchanged 3 times at 80 ℃ of ammonium nitrate solutions with 0.8mol/L, wash 2 times, 120 ℃ of dry 10h, obtain ammonia type molecular sieve.By the molecular sieve carried Co of incipient impregnation normal direction ammonia type and Ni metal species, load capacity is 1.5wt%, leaves standstill afterwards 4h, 120 ℃ of dry 10h, and 550 ℃ of roasting 4h, make catalyst, are designated as catalyst I.
[embodiment 8]
The catalytic performance examination of comparative example 1～2 and embodiment 1～7
Catalyst performance examination is carried out on fixed-bed reactor, adopts the stainless steel reactor that internal diameter is 10mm, loaded catalyst 10mL, 520 ℃ of reaction temperatures, synthesis under normal pressure, mass space velocity 5h
-1, raw material adopts the mixed C 5 that is rich in alkene, specifically forms in table 1.Product is analyzed respectively after gas-liquid separation, and gas-phase product adopts Agilent gas-chromatography 6820, Al
2o
3pillar, hydrogen flame detector; Liquid product adopts Agilent gas-chromatography 6820, FFAP pillar, hydrogen flame detector.Analysis result normalization.When being 20h and 60h, reaction time the results are shown in Table 2.Therefrom can find out, compare with B with the catalyst A of non-modified have small size raising through the upper mixed C 5 raw material initial conversion of the catalyst C-I of alkali treatment modifying load different content metallic element and aromatics yield, reaction stability has obtained and has significantly improved.
Table 1 mixed C 5 olefin feedstock compositions
| Raw material components | Pentane | Isopentane | Positive amylene | Iso-amylene |
| Percentage composition (wt%) | 17.4 | 2.8 | 16.3 | 63.5 |
Table 2 mixed C 5 alkene aromatized catalyst performance evaluation results
[embodiment 9]
Catalyst stability examination
On the device of [embodiment 8], adopt respectively the mixed C 5 (composition is in table 3) that is rich in the mixed C 5 (composition is in table 1) of alkene and is rich in alkane, as raw material, catalyst H is carried out to stability examination, examination condition is: synthesis under normal pressure, mass space velocity 0.6h
-1, 520～540 ℃ of reaction temperatures.Appraisal result is in table 4.Therefrom can find out, in the time that the mixed C 5 that is rich in alkene is made raw material, catalyst single pass life reaches 700h, aromatics yield 49wt%; In the time that the mixed C 5 that is rich in alkane is made raw material, catalyst single pass life reaches 1000h, and aromatics yield 38wt% shows that catalyst is keeping under the prerequisite of aromatization activity, and reaction stability is significantly improved.
Table 3 mixes C 5 alkane composition
| Raw material components | Normal butane | Pentane | Isopentane | N-hexane | Isohexane | Cycloalkane | Alkene |
| Percentage composition (wt%) | 3.9 | 25.9 | 44.0 | 4.2 | 12.5 | 8.6 | 0.9 |
Table 4 catalyst life appraisal result
Claims (1)
1. a preparation method for C5 hydrocarbon aromatization catalyst, step is as follows:
To remove the NaZSM-5 molecular sieve of template and boehmite, field mountain valley with clumps of trees and bamboo powder according to weight ratio ZSM-5: Al
2o
3: mountain valley with clumps of trees and bamboo powder=1, field: mix at 0.3: 0.1; In mixture, add appropriate salpeter solution, pinch even and extruded moulding, in 120 ℃ of dry 10h, 550 ℃ of roasting 3h, pelletizing; Molecular sieve 20g after moulding is placed in to the NaOH solution of 200mL, 0.3M, 70 ℃ of waters bath with thermostatic control are also stirred 5h, and cool to room temperature filters, washs to neutral; Afterwards resulting materials is exchanged 3 times at 80 ℃ of ammonium nitrate solutions with 0.8mol/L, wash 2 times, 120 ℃ of dry 10h, obtain ammonia type molecular sieve; By the molecular sieve carried Ni of incipient impregnation normal direction ammonia type, Zn and Fe metal species, load capacity is 1.0wt%, leaves standstill afterwards 4h, 120 ℃ of dry 10h, and 550 ℃ of roasting 4h, make catalyst.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1341699A (en) * | 2000-09-06 | 2002-03-27 | 中国石油化工集团公司 | Low-carbon hydrocarbon aromatization method |
| CN101352689A (en) * | 2007-07-25 | 2009-01-28 | 中国科学院大连化学物理研究所 | Modification method of molecular sieve catalyst for hexene aromatization reaction |
| CN101530813A (en) * | 2008-03-12 | 2009-09-16 | 中国科学院大连化学物理研究所 | Method for preparing molecular sieve catalyst used in carbon 4 liquid gas aromatization reaction |
| CN101580737A (en) * | 2008-05-16 | 2009-11-18 | 中国科学院大连化学物理研究所 | Preparation method of molecular sieve catalyst for milling aromatization reaction of distilled gasoline and liquefied gas |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1341699A (en) * | 2000-09-06 | 2002-03-27 | 中国石油化工集团公司 | Low-carbon hydrocarbon aromatization method |
| CN101352689A (en) * | 2007-07-25 | 2009-01-28 | 中国科学院大连化学物理研究所 | Modification method of molecular sieve catalyst for hexene aromatization reaction |
| CN101530813A (en) * | 2008-03-12 | 2009-09-16 | 中国科学院大连化学物理研究所 | Method for preparing molecular sieve catalyst used in carbon 4 liquid gas aromatization reaction |
| CN101580737A (en) * | 2008-05-16 | 2009-11-18 | 中国科学院大连化学物理研究所 | Preparation method of molecular sieve catalyst for milling aromatization reaction of distilled gasoline and liquefied gas |
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