CN106582775A - Catalyst for preparing isobutene - Google Patents
Catalyst for preparing isobutene Download PDFInfo
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Abstract
The invention relates to a catalyst for preparing isobutene, a preparation method for the catalyst and an application of the catalyst. The catalyst is mainly used for solving the problem in the prior art that the catalyst stability is poor. According to the catalyst, through adopting the technical scheme that the catalyst for preparing the isobutene through dehydrogenating isobutane contains a carrier, an active ingredient and auxiliaries, wherein at least one of MCF and SAPO serve as the carrier, vanadium serves as the active ingredient, and one or more of Sb and rare-earth metal serve as the auxiliaries, the technical problem is better solved, so that the catalyst can be applied to the industrial production of preparation of the isobutene through dehydrogenating the isobutane in a carbon dioxide atmosphere.
Description
Technical field
The present invention relates to a kind of catalyst for preparing isobutene., preparation method and applications.
Background technology
Isobutene. is a kind of very important industrial chemicals, in Chemical Manufacture, the purposes of isobutene. widely,
Can be used to synthesizing methyl tertbutyl ether (MTBE), ethyl tert-butyl oxide (ETBE), butyl rubber, ABS
Resin etc..With the production-scale expansion of isobutene. downstream product, the demand of isobutene. also constantly increases.
The isobutene. amount that traditional method is obtained can not meet the demand in market.In addition, the C4 resources of China are very rich
Richness, but compared with American-European countries China C4 resource utilizations than relatively low less than 40%, only American-European countries
Half or so, and be concentrated mainly in the utilization of alkene, most alkane is used as fuel, brings greatly money
Source wastes.The isobutene. that the dehydrogenation of isobutane of relative low price produces high added value can be solved into isobutene.
Shortage can produce bigger economic benefit again.
Preparing isobutene through dehydrogenation of iso-butane is broadly divided into catalytic dehydrogenation, dioxygen oxidation dehydrogenation and carbon dioxide atmosphere dehydrogenation
Three kinds of methods.Catalytic dehydrogenation of isobutane has realized at present industrialization, but the reaction is limited by thermodynamical equilibrium,
And observable index is larger.The dehydrogenation of iso-butane dioxygen oxidation can bring deep oxidation, and products distribution is uncontrolled, causes
The low problem of selectivity.Preparing isobutene through dehydrogenation of iso-butane combines catalytic dehydrogenation and oxygen oxygen under carbon dioxide atmosphere
The advantage of fluidized dehydrogenation, is a kind of new method with potential competition ability.Carbon dioxide can be with dehydrogenation generation
There is inverse water gas reaction in hydrogen, limit so as to break thermodynamical equilibrium, dehydrogenation reaction is moved to product；Or
Person's carbon dioxide directly can occur oxidative dehydrogenation with iso-butane.Above two mechanism can improve isobutyl
The equilibrium conversion of alkane.Additionally, carbon dioxide is changed into during the course of the reaction more as main greenhouse gases
For active and be industrially easier the carbon monoxide for utilizing, greenhouse emissions not only reduced but also have taken full advantage of carbon money
Source, with certain social value.
Carbon dioxide atmosphere preparing isobutene through dehydrogenation of iso-butane is extensively taken seriously, for example, Ogonowski classes
Topic group VMgO catalyst, when reaction temperature is 600 DEG C, conversion ratio is 13%, and selectivity is 80%
(Catalysis Communications, 2009 volume 11 page 132～136).Chinese patent CN
102631914A is prepared for the vanadium pentoxide catalyst that mesoporous carbon is carrier, is 610 DEG C of bars in reaction temperature
The conversion ratio of iso-butane is about 32% under part, and selectivity is about 91.4%.Shimada et al. is negative using activated carbon
The ferric oxide catalyst of load, reaction temperature is that the conversion ratio of iso-butane under the conditions of 600 DEG C is about 23%, selectivity
About 80%, and catalyst inactivation is fast, iso-butane conversion ratio is down to 13% (Applied after reacting 3 hours
Catalysis A:General, 1998 volume 168 page 243～250).It can be seen that, catalyst is with the response time
Prolongation, activity occurs decline, raising prepare the stability of isobutene catalyst be urgent need to resolve problem it
One.
The content of the invention
One of the technical problem to be solved is the problem of poor catalyst stability in prior art, there is provided
A kind of catalyst of new preparing isobutene through dehydrogenation of iso-butane.The characteristics of catalyst has good stability.
The two of the technical problem to be solved in the present invention be to provide it is a kind of with solve that one of technical problem is corresponding to urge
Agent preparation method.
The three of the technical problem to be solved in the present invention are to provide a kind of answering for the catalyst of one of solution technical problem
With.
To solve one of above-mentioned technical problem, the technical solution used in the present invention is as follows：Prepare the catalysis of isobutene.
Agent, including carrier, active component and auxiliary agent, described catalyst with MCF, SAPO molecular sieve at least
One kind be carrier, with vanadium as active component, with Sb and rare earth metal one or more as auxiliary agent.
In above-mentioned technical proposal, in terms of the stability of catalyst is promoted, in the auxiliary agent between Sb and rare earth
With mutual promoting action, the facilitation between such as but not limited to Sb and Ce.
Described rare earth metal is not particularly limited, La such as but not limited in light rare earth metal element, Ce,
Pr, Nd, Pm etc..But it is preferred that the rare earth includes Ce and Nd simultaneously, now catalyst has preferably stable
Property while, both are with synergism in terms of activity is improved.
In above-mentioned technical proposal, the weight/mass percentage composition of vanadium is preferably 0.6～29%, more preferably 1 in terms of V2O5
～10%.
In above-mentioned technical proposal, the weight/mass percentage composition of Sb is preferably 0.1～5% in terms of Sb2O5
In above-mentioned technical proposal, the weight/mass percentage composition of rare earth metal is preferably in terms of the trivalent of rare earth
0.3～5.0%.
To solve the two of above-mentioned technical problem, the technical solution used in the present invention is as follows：One of above-mentioned technical problem
Technical scheme described in catalyst preparation method, comprise the following steps：
1) aequum carrier is successively mixed with the solution containing vanadium and the solution containing auxiliary agent, or by aequum carrier
Mix with the solution simultaneously containing vanadium and containing auxiliary agent；
2) roasting obtains the catalyst.
In above-mentioned technical proposal, described solution preferably adopts the solvent of water, one skilled in the art will appreciate that root
According to vanadium-containing compound and the property containing auxiliary compound, pH is adjusted so that above-claimed cpd is dissolved in acid or alkali
Solution is formed in water.
Carrier can successively mix with the solution containing vanadium and the solution containing auxiliary agent, and sequencing is not limited, or
Mix with the mixed solution simultaneously containing vanadium and containing auxiliary agent.
Using carrier with containing vanadium and during solution hybrid mode containing auxiliary agent, the preparation method of mixed solution can be but
It is not limited to：
A, the tartaric acid by the compound dissolution of the desired amount of vanadium with 0.25 appropriate mol/L in water are water-soluble
Liquid is dissolved in beaker, obtains the aqueous solution containing vanadium；
B, the desired amount of antimony and rare earth compound are added in the aqueous solution containing vanadium in step a, stirring and dissolving,
The aqueous solution of vanadium and auxiliary agent must be contained；
In above-mentioned technical proposal, the compound of vanadium is not particularly limited, such as but not limited to ammonium metavanadate, sulphuric acid
One kind of vanadyl and vanadyl oxalate, the compound of antimony is not particularly limited, such as but not limited to chlorate, described
Rare earth compound is it is not also specifically limited, such as but not limited to nitrate, chloride etc..
In above-mentioned technical proposal, sintering temperature is preferably 550～850 DEG C, more preferably 600～700 DEG C.
In above-mentioned technical proposal, roasting time is preferably 2～10 hours, more preferably 4～6 hours.
In above-mentioned technical proposal, one skilled in the art will appreciate that being preferably step 1) and step 2) between
With dry step.
In above-mentioned technical proposal, dry temperature is preferably 90～140 DEG C.
In above-mentioned technical proposal, Ce is often present in the form of ceo 2 in final catalyst, other rare earth metals
Often in the form of trivalent.
To solve the three of above-mentioned technical problem, the technical solution used in the present invention is as follows：Above-mentioned catalyst is applied to
Under carbon dioxide atmosphere in the reaction of preparing isobutene through dehydrogenation of iso-butane.
In above-mentioned technical proposal, preferably carbon dioxide is 1～10 with the mol ratio of iso-butane.
In above-mentioned technical proposal, the temperature of reaction is preferably 550～640 DEG C.
In above-mentioned technical proposal, the mass space velocity of iso-butane 0.1～3 hour -1.
Iso-butane conversion ratio, active reduction rate are calculated as follows：
Active reduction rate is bigger, illustrates that catalyst is more unstable, and vice versa.The explanation when this value is negative
Activity goes up not down, then be more favorable result.
Under the experiment condition of the present invention, preparing the catalyst of isobutene. can continuously run 8h to the present invention, tool
There is preferable stability, achieve preferable technique effect.
Below by embodiment, the invention will be further elaborated：
Specific embodiment
【Embodiment 1】
1st, catalyst preparation
Will be equivalent to the ammonium metavanadate of 8 grams of V2O5, the cerous nitrate equivalent to 2.5 grams of CeO2 and equivalent to
The Butter of antimony. of 3.0 grams of Sb2O5 is dissolved in the aqueous tartaric acid solution of 40 milliliter of 0.25 mol/L, with 86.5
The mixing of gram MCF carriers, stands 8 hours at room temperature, then at 120 DEG C of dryings 24 hours, most after 620 DEG C
Catalyst needed for roasting is obtained for 6 hours in muffle furnace, for ease of comparing, by the composition of catalyst table 1 is listed in.
2nd, evaluating catalyst
As stated above obtained catalyst carries out activity rating in fixed bed reactors, and process is as follows：
The internal diameter of reactor is 8 millimeters of stainless steel tube, long 400 millimeters.Carbon dioxide and iso-butane mol ratio
For 5.0, reaction temperature is 575 DEG C, and the mass space velocity of iso-butane is 0.8 hour -1, and reaction pressure is normal pressure.
For ease of comparing, catalyst activity evaluation the results are shown in Table 2.
【Comparative example 1】
1st, catalyst preparation
The ammonium metavanadate and the cerous nitrate equivalent to 5.5 grams of CeO2 that will be equivalent to 8 grams of V2O5 is dissolved in 40 millis
In rising the aqueous tartaric acid solution of 0.25 mol/L, mix with 86.5 grams of MCF carriers, 8 are stood at room temperature
Hour, then at 120 DEG C of dryings 24 hours, catalysis needed for roasting is obtained for 6 hours most in 620 DEG C of muffle furnaces
Agent, for ease of comparing, by the composition of catalyst table 1 is listed in.
2nd, evaluating catalyst
As stated above obtained catalyst carries out activity rating in fixed bed reactors, and process is as follows：
The internal diameter of reactor is 8 millimeters of stainless steel tube, long 400 millimeters.Carbon dioxide and iso-butane mol ratio
For 5.0, reaction temperature is 575 DEG C, and the mass space velocity of iso-butane is 0.8 hour -1, and reaction pressure is normal pressure.
For ease of comparing, catalyst activity evaluation the results are shown in Table 2.
【Comparative example 2】
1st, catalyst preparation
The ammonium metavanadate and the Butter of antimony. equivalent to 5.5 grams of Sb2O5 that will be equivalent to 8 grams of V2O5 is dissolved in 40
In the aqueous tartaric acid solution of 0.25 mol/L of milliliter, mix with 86.5 grams of MCF carriers, 8 are stood at room temperature
Hour, then at 120 DEG C of dryings 24 hours, catalysis needed for roasting is obtained for 6 hours most in 620 DEG C of muffle furnaces
Agent, for ease of comparing, by the composition of catalyst table 1 is listed in.
2nd, evaluating catalyst
As stated above obtained catalyst carries out activity rating in fixed bed reactors, and process is as follows：
The internal diameter of reactor is 8 millimeters of stainless steel tube, long 400 millimeters.Carbon dioxide and iso-butane mol ratio
For 5.0, reaction temperature is 575 DEG C, and the mass space velocity of iso-butane is 0.8 hour -1, and reaction pressure is normal pressure.
For ease of comparing, catalyst activity evaluation the results are shown in Table 2.
【Embodiment 2】
1st, catalyst preparation
Will be equivalent to the ammonium metavanadate of 8 grams of V2O5, the neodymium nitrate equivalent to 2.5 grams of Nd2O3 and equivalent to
The Butter of antimony. of 3.0 grams of Sb2O5 is dissolved in the aqueous tartaric acid solution of 40 milliliter of 0.25 mol/L, with 86.5
The mixing of gram MCF carriers, stands 8 hours at room temperature, then at 120 DEG C of dryings 24 hours, most after 620 DEG C
Catalyst needed for roasting is obtained for 6 hours in muffle furnace, for ease of comparing, by the composition of catalyst table 1 is listed in.
2nd, evaluating catalyst
As stated above obtained catalyst carries out activity rating in fixed bed reactors, and process is as follows：
The internal diameter of reactor is 8 millimeters of stainless steel tube, long 400 millimeters.Carbon dioxide and iso-butane mol ratio
For 5.0, reaction temperature is 575 DEG C, and the mass space velocity of iso-butane is 0.8 hour -1, and reaction pressure is normal pressure.
For ease of comparing, catalyst activity evaluation the results are shown in Table 2.
【Embodiment 3】
1st, catalyst preparation
Will be equivalent to the ammonium metavanadate of 8 grams of V2O5, the neodymium nitrate equivalent to 1.0 grams of Nd2O3, equivalent to
The cerous nitrate of 1.5 grams of CeO2 and the Butter of antimony. equivalent to 3.0 grams of Sb2O5 are dissolved in 40 milliliter 0.25 and rub
You/liter aqueous tartaric acid solution in, mix with 86.5 grams of MCF carriers, at room temperature standing 8 hours, then at
120 DEG C of dryings 24 hours, catalyst needed for roasting is obtained for 6 hours most in 620 DEG C of muffle furnaces, for ease of
Relatively, the composition of catalyst is listed in into table 1.
2nd, evaluating catalyst
As stated above obtained catalyst carries out activity rating in fixed bed reactors, and process is as follows：
The internal diameter of reactor is 8 millimeters of stainless steel tube, long 400 millimeters.Carbon dioxide and iso-butane mol ratio
For 5.0, reaction temperature is 575 DEG C, and the mass space velocity of iso-butane is 0.8 hour -1, and reaction pressure is normal pressure.
For ease of comparing, catalyst activity evaluation the results are shown in Table 2.
【Embodiment 4】
1st, catalyst preparation
Will be equivalent to the ammonium metavanadate of 8 grams of V2O5, the praseodymium nitrate equivalent to 2.5 grams of Pr2O3 and be dissolved in 25
In the oxalic acid aqueous solution of 0.25 mol/L of milliliter, mix with 90 grams of SBA-15 carriers, 4 are stood at room temperature
Hour, then at 100 DEG C of dryings 24 hours, catalysis needed for roasting is obtained for 4 hours most in 600 DEG C of muffle furnaces
Agent, for ease of comparing, by the composition of catalyst table 1 is listed in.
2nd, evaluating catalyst
As stated above obtained catalyst carries out activity rating in fixed bed reactors, and process is as follows：
The internal diameter of reactor is 8 millimeters of stainless steel tube, long 400 millimeters.Carbon dioxide and iso-butane mol ratio
For 5.0, reaction temperature is 590 DEG C, and the mass space velocity of iso-butane is 1.0 hours -1, and reaction pressure is normal pressure.
For ease of comparing, catalyst activity evaluation the results are shown in Table 2.
【Embodiment 5】
1st, catalyst preparation
Will be equivalent to the ammonium metavanadate of 8 grams of V2O5, the Lanthanum (III) nitrate equivalent to 2.5 grams of La 2O3 and equivalent to
The Butter of antimony. of 3.0 grams of Sb2O5 is dissolved in the aqueous tartaric acid solution of 40 milliliter of 0.25 mol/L, with 86.5
The mixing of gram MCF carriers, stands 8 hours at room temperature, then at 120 DEG C of dryings 24 hours, most after 620 DEG C
Catalyst needed for roasting is obtained for 6 hours in muffle furnace, for ease of comparing, by the composition of catalyst table 1 is listed in.
2nd, evaluating catalyst
As stated above obtained catalyst carries out activity rating in fixed bed reactors, and process is as follows：
The internal diameter of reactor is 8 millimeters of stainless steel tube, long 400 millimeters.Carbon dioxide and iso-butane mol ratio
For 5.0, reaction temperature is 575 DEG C, and the mass space velocity of iso-butane is 0.8 hour -1, and reaction pressure is normal pressure.
For ease of comparing, catalyst activity evaluation the results are shown in Table 2.
【Embodiment 6】
1st, catalyst preparation
Will be equivalent to the ammonium metavanadate of 29 grams of V2O5, the cerous nitrate equivalent to 1.0 grams of CeO2 and equivalent to
The Butter of antimony. of 0.5 gram of Sb2O5 is dissolved in the aqueous tartaric acid solution of 45 milliliter of 0.25 mol/L, with 69.5
The mixing of gram MCF carriers, stands 8 hours at room temperature, then at 90 DEG C of dryings 36 hours, most after 800 DEG C
Catalyst needed for roasting is obtained for 2 hours in muffle furnace.
2nd, evaluating catalyst
As stated above obtained catalyst carries out activity rating in fixed bed reactors, and process is as follows：
The internal diameter of reactor is 8 millimeters of stainless steel tube, long 400 millimeters.Carbon dioxide and iso-butane mol ratio
For 2.0, reaction temperature is 640 DEG C, and the mass space velocity of iso-butane is 1.0 hours -1, and reaction pressure is normal pressure.
Reaction result is：When response time is 30 minutes, iso-butane conversion ratio is 30.6%；Response time is 8
After hour, iso-butane conversion ratio is 29.1%.
【Embodiment 7】
1st, catalyst preparation
Will be equivalent to the ammonium metavanadate and the cerous nitrate equivalent to 5 grams of CeO2 of 1 gram of V2O5 and equivalent to 5
The Butter of antimony. of gram Sb2O5 is dissolved in the aqueous tartaric acid solution of 45 milliliter of 0.25 mol/L, with 89 grams
SAPO-34 carriers mix, and stand 8 hours at room temperature, then at 150 DEG C of dryings 24 hours, most after 580 DEG C
Catalyst needed for roasting is obtained for 10 hours in muffle furnace.
2nd, evaluating catalyst
As stated above obtained catalyst carries out activity rating in fixed bed reactors, and process is as follows：
The internal diameter of reactor is 8 millimeters of stainless steel tube, long 400 millimeters.Carbon dioxide and iso-butane mol ratio
For 10.0, reaction temperature is 550 DEG C, and the mass space velocity of iso-butane is 1.0 hours -1, and reaction pressure is normal pressure.
Reaction result is：When response time is 30 minutes, iso-butane conversion ratio is 28.1%；Response time is 8
After hour, iso-butane conversion ratio is 27.5%.
Table 1
| V2O5 | Sb2O5 | Nd2O3 | CeO2 | Pr2O3 | La2O3 | Carrier | |
| Embodiment 1 | 8 | 3.0 | - | 2.5 | - | - | 86.5 |
| Comparative example 1 | 8 | - | - | 5.5 | - | - | 86.5 |
| Comparative example 2 | 8 | 5.5 | - | - | - | - | 86.5 |
| Embodiment 2 | 8 | 3.0 | 2.5 | - | - | - | 86.5 |
| Embodiment 3 | 8 | 3.0 | 1.0 | 1.5 | - | - | 86.5 |
| Embodiment 4 | 8 | 3.0 | - | - | 2.5 | - | 86.5 |
| Embodiment 5 | 8 | 3.0 | - | - | - | 2.5 | 86.5 |
Note：Catalyst composition is represented with weight percentage in table 1.
Table 2
Claims (10)
1. the catalyst of isobutene., including carrier, active component and auxiliary agent are prepared, it is characterised in that：Described urges
Agent with least one in MCF, SAPO molecular sieve as carrier, with vanadium as active component, with Sb and rare earth
One or more of metal are auxiliary agent.
2. catalyst according to claim 1, it is characterised in that the weight/mass percentage composition of vanadium is with V2O5It is calculated as
0.6～29%.
3. catalyst according to claim 1, it is characterised in that the weight/mass percentage composition of Sb is with Sb2O5It is calculated as
0.1～5%.
4. catalyst according to claim 1, it is characterised in that the weight/mass percentage composition of rare earth metal is with rare earth
Trivalent is calculated as 0.3～5.0%.
5. the preparation method of the catalyst described in claim 1, comprises the following steps：
1) aequum carrier is successively mixed with the solution containing vanadium and the solution containing auxiliary agent, or by aequum carrier with it is same
When containing vanadium and containing auxiliary agent solution mixing；
2) roasting obtains the catalyst.
6. preparation method according to claim 5, it is characterised in that sintering temperature is 550～850 DEG C.
7. preparation method according to claim 5, it is characterised in that when roasting time is roasting in 2～10 hours
Between.
8. preparation method according to claim 5, it is characterised in that step 1) and step 2) between have
Dry step.
9. preparation method according to claim 8, it is characterised in that dry temperature is 90～140 DEG C.
10. the catalyst described in claim 1 is applied to the reaction of preparing isobutene through dehydrogenation of iso-butane under carbon dioxide atmosphere
In.
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-
2015
- 2015-10-16 CN CN201510672575.2A patent/CN106582775B/en active Active
Patent Citations (4)
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| CN101773850A (en) * | 2010-01-28 | 2010-07-14 | 清华大学 | Catalyst for manufacturing olefin by low-carbon alkane dehydrogenation and application thereof |
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