CN104923285A - Catalyst for preparing hydrocarbons from oxygen-containing compounds, and preparation method and application thereof - Google Patents
Catalyst for preparing hydrocarbons from oxygen-containing compounds, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a catalyst for preparing hydrocarbons from oxygen-containing compounds, and a preparation method and application thereof. The catalyst, on a basis of total weight, comprises 35-84% of ZSM-5 molecular sieve, 15-60% of a binder and 0.1- 15% of modified elements. The catalyst is prepared by preparing modified ZSM-5 molecular sieve, mixing the ZSM-5 molecular sieve with the binder and performing extrusion molding, and post-processing. The catalyst is used for preparing hydrocarbons from oxygen-containing compounds, is high in catalytic activity, good in hydrocarbon selectivity, long in single pass life and simple in preparation process.
Description
Technical field
The present invention relates to a kind of catalyst of oxygenatedchemicals hydrocarbon, particularly a kind of catalyst and preparation method and application oxygenatedchemicals being converted into hydrocarbon.
Technical background
Along with the development of Coal Chemical Industry, synthesis and the transformation technology of coal-based oxygenatedchemicals are more and more ripe, in recent years in order to enhance competitiveness, China's oxygenatedchemicals is produced towards maximization, energy-saving development, coal-based oxygenatedchemicals accounts for more than 80% of oxygenatedchemicals output, oxygenatedchemicals output increases year by year, and then there is serious problem of excess production capacity, end in November, 2012, the oxygenatedchemicals manufacturing enterprise 172 of the total production capacity more than 100,000 tons/year of China, production capacity adds up to 5,050 ten thousand tons/year.China's oxygenatedchemicals output 1984.1 ten thousand tons in 2011, the industry utilization of capacity is about 41%.Estimate that China's methanol output in 2012 is 2,600 ten thousand tons, the industry utilization of capacity 51%.The oxygenatedchemicals hydrocarbon market space is large, there is the oxygenatedchemicals downstream project of large-scale production and high added value, also be that oxygenatedchemicals industry is extricated oneself from a predicament, step into the outlet of benign development, therefore the exploitation actively carrying out oxygenatedchemicals downstream product has very important meaning to oxygenatedchemicals industrial expansion, the exploitation of its key technology is exactly suitable catalyst development.
Preparing gasoline by methanol (MTG) technique refers to methyl alcohol to be raw material, under uniform temperature, pressure and air speed, with specific catalyst carry out dewatering, the step such as oligomeric, isomery is converted into the process that carbon number is less than 11 hydrocarbon-type oils.1976, Mobil company becomes in the technical foundation of aromatic hydrocarbons in its methanol conversion, have developed MTG technology, main-process stream is for synthesis gas produced by raw material with coal or natural gas, use synthesising gas systeming carbinol again, finally crude carbinol is converted into high-knock rating gasoline, used catalyst is the ZSM-5 catalyst of Mobil company research and development.
Methanol aromatic hydrocarbons (MTA) theory appears in the MTG technology of Mobil company exploitation the earliest, 20 century 70 Mobil companies develop ZSM-5 zeolite molecular sieve, utilize this zeolite molecular sieve to be high-knock rating gasoline by methanol conversion effectively, wherein arene content is greater than 35%.Subsequently Mobil company at U. S. application patent USP4590321, disclose the experimental result of Methanol aromatic hydrocarbons, this patent Introduction adopts the ZSM-5 zeolite molecular sieve of P modification to be catalyst, and P content is 2.7%, reaction temperature is between 400 ~ 450 DEG C, and methanol feeding air speed is 1.3h
-1, the ZSM-5 molecular sieve catalyst of experimental result display P modification at higher hydrocarbon, aromatic hydrocarbons selective on well more a lot of than unmodified ZSM-5 molecular sieve, but arene content is not very high.Subsequently, Mobil company has applied for again US Patent No. P4686312, and disclosing low-carbon oxygen-containing converting compounds such as methyl alcohol is the multistage reaction process of the product being rich in aromatic hydrocarbons.Be low-carbon alkanes and alkene in first paragraph methanol conversion, enter second segment reactor subsequently, under the effect of catalyst, further aromatization occurs, obtain the product being rich in low-carbon (LC) aromatic hydrocarbons.
Patent CN1880288A discloses a kind of process of methanol conversion for preparing arene and catalyst and method for preparing catalyst, the percentage by weight of its first paragraph catalyst consists of: little crystal grain HZSM-5-62.0-85.0, Ga-0.5 ~ 2.0, La-0.2 ~ 1.0, binding agent 14.0 ~ 34.0.Second segment catalyst feature is that the mol ratio of silicon gallium is 63 ~ 218, lanthanum content is 0.83 ~ 2.12wt%, total acid content is that the catalyst of 0.468 ~ 0.672mmol/g.cat activates 1 ~ 20 hour in 360 ~ 480 DEG C of high-temperature water vapors, makes catalyst be 0.073 ~ 0.079g/g catalyst to the static adsorbance of cyclohexane.
The article " the HZSM-5 molecular sieve aromatization of methanol catalyst reaction performance of Ga modification " that the researchers such as Liu Weiqiao deliver in the 30th volume the 12nd phase in 2011 " chemical industry progress " specifically understands in infusion process and Hydrothermal Synthesis normal direction HZSM-5 introduces the impact of Ga on aromatization of methanol performance, experimental result shows, adopt and introduce Ga in two ways later to catalyst crystal structure, aperture and pattern affect all very little, and it is larger on acidic zeolite impact, the activity of the raising catalyst that the Ga that Hydrothermal Synthesis is introduced can follow and arenes selectivity, in addition, the introducing of Ga can suppress the carbon distribution of catalyst effectively.
The researchers such as Sheng Qingtao were at the 43rd volume in 2012, publish an article in 4th phase " Institutes Of Technology Of Taiyuan's journal " " steam and HCl treatment are on the impact of ZSM-5 molecular sieve performance " specifically understand that steam treatment and HCl treatment are on the impact of catalyst performance, experimental result shows, steam treatment makes ZSM-5 molecular sieve generation framework dealumination, acid site quantity reduces, acid strength weakens, but catalyst is mesoporous increases, thus catalyst stability is improved.
The researchers such as Zhao Yonghua publish an article in " petroleum refining and the chemical industry " of the 40th volume 11 phase in 2009 " silanization treatment is on the impact of HZSM-5 molecular sieve Aromatization Activity " specifically understand silanization treatment on the impact of HZSM-5 catalyst.Experimental result shows the increase along with silane contents, and molecular sieve surface L acid there is no change, and B acid number amount reduces gradually, and in liquid-phase product, arene content improves gradually, and molecular sieve catalyst stability improves.
The researchers such as Fang Yiwen publish an article " the dimethyl ether aromatization on Zn/HZSM-5 catalyst " detailed dimethyl ether Aromatization Activity describing the HZSM-5 catalyst of Zn modification on " the catalysis journal " of the 31st volume 3 phase in 2012, experimental result shows that the introducing of Zn can increase acid intensity in HZSM-5 and acid site, and these are all conducive to dimethyl ether aromatisation.
The researchers such as Miao Xingdong publish an article in " research and development " " hydrothermal treatment consists temperature is on the impact of Zn-P/HZSM-5 catalyst Aromatization Activity ", what it was detailed describes the impact of hydrothermal treatment consists temperature on HZSM-5 catalyst performance, experimental result shows, hydrothermal treatment consists can improve the stability of Zn-P/ZSM-5 zeolite, modulation acidity and pore passage structure, and, along with the raising of hydrothermal treatment consists temperature, the total acid content of zeolite declines, and strong acid declines faster, but high temperature has larger destruction to zeolite crystallinity.
Tian Tao, the researchers such as Wei Fei published an article " on Ag/ZSM-5 catalyst aromatization of methanol process " in 2009 in the 29th volume the 1st phase " modern chemical industry ", what this paper was detailed has investigated reaction temperature, acidity of catalyst, methanol partial pressure and Ag pickup are on the impact of aromatization of methanol reaction selectivity, high methanol partial pressure is conducive to improving arenes selectivity, and significantly changes aromatic hydrocarbon product composition, and arenes selectivity raised along with the rising of reaction temperature and silver content before this.
The people such as Bjorgen find that alkali treatment can improve the suppression carbon distribution deactivation of molecular sieve, this molecular sieve analog processing method is introduced in the reaction of Methanol hydro carbons, not only can improve the activity of catalyst, improve the selective of hydrocarbon product, the most important thing is the stability that can significantly improve catalyst, improve the life-span of catalyst.But about the committed step of molecular sieve alkali treatment process, the relation between alkali treatment condition and commercial performance does not also have systematic account at present.
Summary of the invention
The invention provides the catalyst that a kind of oxygenatedchemicals produces hydrocarbon, this catalyst is a kind of long-life, and efficient oxygenatedchemicals produces long chain hydrocarbon catalyst.On the catalyst, oxygenatedchemicals is converted into hydrocarbon compound by a step, and this catalyst activity is high, and single pass life is long, and hydrocarbon-selective is high.
Present invention also offers the preparation method that a kind of oxygenatedchemicals produces the catalyst of hydrocarbon.
Present invention also offers the application that a kind of oxygenatedchemicals produces hydrocarbon catalyst.
The catalyst of a kind of oxygenatedchemicals hydrocarbon of the present invention, comprises the ZSM-5 molecular sieve of 35 ~ 84%, the binding agent of 15 ~ 60% and the modifying element of 0.1 ~ 15%, and preferably 0.4 ~ 10%, with overall catalyst weight gauge.
Oxygenatedchemicals of the present invention is at least one in methyl alcohol, dimethyl ether.
Hydrocarbon of the present invention is C
1~ C
15hydrocarbon, preferred C
4~ C
11hydrocarbon.
Described binding agent is the one in SB powder or boehmite.
The 8iO of described ZSM-5 molecular sieve
2/ Al
2o
3mol ratio is 38 ~ 120, preferably 38 ~ 90.
Described modifying element is at least Zn, the one in P, La, Fe, preferred Zn.
Described catalyst is bar shaped, ball-type, trifolium-shaped, bunge bedstraw herb type, preferred bar shaped.
A kind of oxygenatedchemicals of the present invention produces the method for preparing catalyst of hydrocarbon, and step is as follows:
1) modified zsm-5 zeolite is prepared, equi-volume impregnating is adopted to be poured into uniformly in ZSM-5 molecular sieve by the nitrate solution of modifying element, after stirring, at room temperature leave standstill 24h, dry at 100 ~ 120 DEG C of temperature, roasting 5h at 500 ~ 550 DEG C, obtains modified ZSM-5 molecular sieve, enters step 2);
2) from step 1) modified zsm-5 zeolite and binding agent kneading extrusion forming, in left at room temperature 24h, at 100 ~ 120 DEG C dry, at 500 ~ 550 DEG C, roasting 5h, obtains catalyst, enters step 3);
3) will from step 2) catalyst load in fixed bed reactors, process successively with sodium hydroxide solution, ammonium nitrate solution and steam, then at 500 ~ 550 DEG C roasting 5h.
Described sodium hydroxide solution treatment conditions are: concentration of sodium hydroxide solution is 0.1 ~ 1.5mol/L, and treatment conditions are temperature 90 ~ 150 DEG C, air speed 3 ~ 20h
-1, the processing time is 0.5 ~ 6h.
Described ammonium nitrate solution treatment conditions are: concentration of ammonium nitrate solution is 0.5 ~ 2.0mol/L, and treatment conditions are air speed 5 ~ 25h
-1, the processing time is 2 ~ 6h.
Described steam treatment condition is: temperature 600 DEG C, steam quality air speed 0.5 ~ 3h
-1, process 6h.
An application for the catalyst of oxygenatedchemicals hydrocarbon, loads catalyst in reactor, at pressure 0.5 ~ 2.5Mpa, under reaction temperature 350 ~ 420 DEG C of conditions, raw material with air speed for 0.6 ~ 5.0h
-1enter reactor to react, be separated product, hydrocarbon liquid phase is product.
Described reactor is fixed bed, fluid bed or moving bed.
Described raw material is methyl alcohol or dimethyl ether.
The advantages such as compared with prior art: the catalyst of a kind of oxygenatedchemicals hydrocarbon of the present invention, have catalyst activity high, hydrocarbon-selective is good, and single pass life is long, and catalyst preparation process is simple, and in alkali treatment ZSM-5 crystallinity loss is little.
Detailed description of the invention
Embodiment 1
The nitrate solution of modifying element Zn is poured in commercially available ZSM-5 molecular sieve, modifying element accounts for 4.0% of catalyst quality, stir, leave standstill 24h, dry at 100 DEG C, at 550 DEG C, roasting 5h obtains modified ZSM-5 molecular sieve, modified molecular sieve and binding agent SB powder kneading extruded moulding, left at room temperature 24h, 100 DEG C of oven dry, roasting 5h at 550 DEG C.Gained strip catalyst is carried out alkali treatment in fixed bed reactors, and naoh concentration used is 0.1mol/L, and treatment conditions are temperature 90 DEG C, sodium hydroxide solution mass space velocity 3h
-1, processing time 6h, change after sodium hydroxide solution is disposed ammonium nitrate solution carry out ammonium exchange process treatment conditions be, concentration of ammonium nitrate solution 0.5mol/L, ammonium nitrate solution weight air speed 5.0h
-1, processing time 6h, exchanges the catalyst of process at 600 DEG C through ammonium nitrate, steam quality air speed 0.5h
-1lower hydrothermal treatment consists 6h, finally namely roasting 5h obtains catalyst of the present invention at 550 DEG C again, and it is 80wt% that catalyst finally consists of ZSM-5 content, and binding agent SB powder content is 16wt%, and modifying element content is 4wt%.
This catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 2 ~ 7
According to the method for embodiment 1, modifying element being accounted for 4.0% of catalyst quality, to change 1%, 2%, 6%, 8%, 10%, ZSM-5 content into constant, and corresponding binder content is that 19%, 18%, 14%, 12%, 10% the other the same as in Example 1 is identical.
Embodiment 8
According to the method for embodiment 1, change binding agent SB powder into boehmite, all the other steps are identical with embodiment 1, and it is 80% that catalyst finally consists of ZSM-5 content, and binding agent boehmite content is 16%, and modifying element content is 4%.
Embodiment 9 ~ 16
According to the method for embodiment 1, change concentration of sodium hydroxide solution used for alkali treatment into 0.2mol/L, 0.4mol/L, 0.6mol/L, 0.8mol/L, 1.0mol/L, 1.1mol/L, 1.2mol/L, 1.5mol/L, all the other steps are identical with embodiment 1, obtain the catalyst that acidity is different with catalyst pore-size distribution, these catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 17 ~ 19
According to the method for embodiment 1, change temperature used for alkali treatment into 100 DEG C, 120 DEG C, 150 DEG C.All the other steps are identical with embodiment 1, obtain the catalyst that acidity is different with catalyst pore-size distribution, these catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 20 ~ 24
According to the method for embodiment 1, change sodium hydroxide solution air speed used for alkali treatment into 5h
-1, 8h
-1, 12h
-1, 16h
-1, 20h
-1, all the other steps are identical with embodiment 1.
Embodiment 25 ~ 29
According to the method for embodiment 1, change utilize the NaOH alkaline solution treatment time used as 5h into, 3h, 2h, 1h, 0.5h, all the other steps are identical with embodiment 1, obtain the catalyst that acidity is different with catalyst pore-size distribution, these catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 30 ~ 32
According to the method for embodiment 1, by ammonium nitrate exchange ammonium nitrate concn change 1.0mol/L into, 1.5mol/L, 2.0mol/L, all the other steps are identical with embodiment 1, obtain catalyst, these catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 33 ~ 36
According to the method for embodiment 1, change the ammonium nitrate solution mass space velocity that ammonium nitrate exchanges into 10h
-1, 15h
-1, 20h
-1, 25h
-1, all the other steps are identical with embodiment 1, obtain catalyst, these catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 37 ~ 39
According to the method for embodiment 1, by ammonium nitrate exchange the ammonium nitrate solution processing time change 5h into, 3h, 2h, all the other steps are identical with embodiment 1, obtain catalyst, these catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 40 ~ 42
According to the method for embodiment 1, change reaction pressure into 1.0Mpa, 1.5Mpa, 2.0Mpa, all the other steps are identical with embodiment 1, obtain catalyst, these catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 43 ~ 46
According to the method for embodiment 1, reaction temperature is changed into 360 DEG C, 380 DEG C, 400 DEG C, 420 DEG C, all the other steps are identical with embodiment 1, to catalyst, these catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 47 ~ 50
According to the method for embodiment 1, change ZSM-5 content in evaluate catalysts into 35%, 45%, 55%, 70%, all the other steps are identical with embodiment 1, obtain catalyst, these catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 51 ~ 56
According to the method for embodiment 1, change evaluate catalysts reaction velocity into 1.0h
-1, 1.5h
-1, 2.5h
-1, 3.0h
-1, 4.0h
-1, 5.0h
-1, all the other steps are identical with embodiment 1, this catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce long chain hydrocarbon reaction, acquired results sees the following form 1.
Embodiment 57
According to the method for embodiment 1, methanol feeding is changed into dimethyl ether charging, all the other steps are identical with embodiment 1, this catalyst at pressure 0.5Mpa, temperature 350 DEG C, air speed 0.6h
-1, methyl alcohol water content is 5%, and carry out methyl alcohol in fixed bed reactors and produce hydrocarbon reaction, acquired results sees the following form 1.
Table 1 each dose of conversion ratio, product yield and catalyst life
Claims (7)
1. a catalyst for oxygenatedchemicals hydrocarbon, comprises the ZSM-5 molecular sieve of 35 ~ 84%, and the binding agent of 15 ~ 60% and the modifying element of 0.1 ~ 15%, with overall catalyst weight gauge.
2. according to the catalyst of a kind of oxygenatedchemicals hydrocarbon according to claim 1, it is characterized in that: described oxygenatedchemicals is at least one in methyl alcohol, dimethyl ether, described hydrocarbon is C
1~ C
15hydrocarbon, described binding agent is the one in SB powder or boehmite, the SiO of described ZSM-5 molecular sieve
2/ Al
2o
3mol ratio is 38 ~ 120, described modifying element is at least Zn, the one in P, La, Fe, accounts for 0.4 ~ 10% of total catalyst weight, and described catalyst is bar shaped, ball-type, trifolium-shaped, bunge bedstraw herb type.
3. according to the catalyst of a kind of oxygenatedchemicals hydrocarbon according to claim 1, it is characterized in that: described catalyst is bar shaped, described hydrocarbon is C
4~ C
11hydrocarbon, described modifying element is the SiO of Zn, described ZSM-5 molecular sieve
2/ Al
2o
3mol ratio is 38 ~ 90.
4. oxygenatedchemicals produces a method for preparing catalyst for hydrocarbon, and step is as follows:
1) modified zsm-5 zeolite is prepared, equi-volume impregnating is adopted to be poured into uniformly in ZSM-5 molecular sieve by the nitrate solution of modifying element, after stirring, at ambient temperature, leave standstill 24h, dry at 100 ~ 120 DEG C of temperature, roasting 5h at 500 ~ 550 DEG C, obtain modified ZSM-5 molecular sieve, enter step 2);
2) from step 1) modified zsm-5 zeolite and binding agent kneading extrusion forming, in left at room temperature 24h, at 100 ~ 120 DEG C dry, at 500 ~ 550 DEG C, roasting 5h, obtains catalyst, enters step 3);
3) will from step 2) catalyst load in fixed bed reactors, process successively with sodium hydroxide solution, ammonium nitrate solution and steam, then at 500 ~ 550 DEG C roasting 5h.
5. produce the preparation method of the catalyst of hydrocarbon according to a kind of oxygenatedchemicals according to claim 4, it is characterized in that: described sodium hydroxide solution treatment conditions are: concentration of sodium hydroxide solution is 0.1 ~ 1.5mol/L, temperature 90 ~ 150 DEG C, air speed 3 ~ 20h
-1, the processing time is 0.5 ~ 6h, and described ammonium nitrate solution treatment conditions are: concentration of ammonium nitrate solution is 0.5 ~ 2.0mol/L, air speed 5 ~ 25h
-1, the processing time is 2 ~ 6h, and described steam treatment condition is: temperature 600 DEG C, air speed 0.5 ~ 3h
-1, process 6h.
6. a catalyst application for oxygenatedchemicals hydrocarbon, loads catalyst in reactor, at pressure 0.5 ~ 2.5Mpa, under reaction temperature 350 ~ 420 DEG C of conditions, raw material with air speed for 0.6 ~ 5.0h
-1enter reactor to react, be separated product, hydrocarbon phase is product.
7. produce the catalyst application of hydrocarbon according to a kind of oxygenatedchemicals according to claim 6, it is characterized in that: described reactor is that fixed bed, fluid bed and moving bed are a kind of.
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| CN114789062A (en) * | 2021-01-25 | 2022-07-26 | 国家能源投资集团有限责任公司 | Modified catalyst and preparation method thereof, and method for producing aromatic hydrocarbon by olefin aromatization |
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Application publication date: 20150923 |