CN104874425A - Modification treatment method of molecular sieve for methanol to gasoline reaction - Google Patents
Modification treatment method of molecular sieve for methanol to gasoline reaction Download PDFInfo
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Abstract
The invention discloses a modification treatment method of a molecular sieve for methanol to gasoline reaction. The method comprises the following steps: mixing and stirring the molecular sieve for methanol to gasoline reaction with an aqueous alkali to obtain a mixture, wherein the aqueous alkali is selected from one or more of Li2CO3, Na2CO3 and K2CO3; transferring the obtained mixture into a high pressure kettle with a polytetrafluoroethylene lining, adding organic amine, sealing, heating and stirring, and then cooling to room temperature, vacuum-filtering, washing to neutral through deionized water, drying at 110 DEG C, passing the night to obtain solid powder; mixing and stirring the obtained solid powder and an acid solution, placing in the high pressure kettle with the polytetrafluoroethylene lining, heating and stirring, and then cooling to room temperature, vacuum-filtering, washing to neutral through the deionized water, drying at 110 DEG C, passing the night, placing in a muffle furnace, calcining at high temperature of 400 DEG C to obtain the modified molecular sieve. Through the adoption of the method disclosed by the invention, the activity, the selectivity and the thermal stability of the molecular sieve are improved.
Description
Technical field
The invention belongs to the catalyst technical field of preparing gasoline by methanol, particularly a kind of modification processing method of the molecular sieve for preparing gasoline by methanol reaction.
Background technology
China's oil resource scarcity, explored oil reserve amount only accounts for 1.4% of world's storage level, but national economy in recent years develop rapidly, energy demand is increased thereupon, also rises year by year to the interdependency of petroleum import.The energy resource structure of China belongs to " rich coal; few oil; deficency "; the storage level of coal resources, output and consumption figure reach 12.6% of world's total amount; 35.3% and 34.4%, therefore the clean conversion of Devoting Major Efforts To Developing coal resources utilizes the study hotspot become instantly and the outlet solving future source of energy crisis.
Coal gasification methanol technics belongs to technique comparatively ripe in the middle of Coal Chemical Industry, and comparatively fast more in China development, and in recent years along with methanol production popularization, downstream methanol outlet is less causes methyl alcohol production capacity surplus.Efforts To Develop methyl alcohol downstream process is developed, and makes full use of the coal resources of China, becomes the important development direction of China's Coal Chemical Industry.
The aluminium that the acid treatment that Chinese patent CN102513142B " a kind of preparation method of preparing gasoline by methanol catalyst " adopts and hydrothermal treatment consists are sloughed on framework of molecular sieve improves silica alumina ratio, the selective of gasoline can be improved, but due to the ZSM-5 molecular sieve that inherently a kind of silicone content higher aluminum content is less, a large amount of pore passage structures sloughing the aluminium atomic destruction molecular sieve on skeleton, certainly will have influence on the long period of activity of molecular sieve.
The employing hydrothermal treatment consists method that Chinese patent CN103506150A " by steam modification for the catalyst of preparing gasoline by methanol and method for making thereof and application " is mentioned to sloughs the unformed aluminium on molecular sieve, dredging duct can be played to a certain extent and increase the effect of specific area, but compared with novel alkaline process process limited use.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of modification processing method of the molecular sieve for preparing gasoline by methanol reaction, the activity of molecular sieve, selective and heat endurance can be improved.
To achieve these goals, the technical solution used in the present invention is:
For a modification processing method for the molecular sieve of preparing gasoline by methanol reaction, comprise the steps:
Step one, by be used for preparing gasoline by methanol reaction molecular sieve and aqueous slkali mix and blend obtain mixture, wherein said aqueous slkali is selected from Li
2cO
3, Na
2cO
3and K
2cO
3in one or more;
Step 2, mixture step one obtained proceed to teflon-lined autoclave, add organic amine, heat stir process 0.5-8h after sealing at 50-200 DEG C;
Step 3, step 2 is heated after mixture be cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, obtain pressed powder;
Step 4, by step 3 gained pressed powder and acid solution mix and blend, be then placed in teflon-lined autoclave, at 50-200 DEG C, heat stir process 0.5-8h;
Step 5, step 4 is heated after mixture be cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve.
Preferably, in described step one, alkaline concentration is 0.1-8mol/L, and the liquid-solid ratio of aqueous slkali and molecular sieve is 10-300ml/g.After molecular sieve mixes with aqueous slkali, stirring at normal temperature 30min.
Preferably, in described step 2, the organic amine added and the mass ratio of molecular sieve are 0.1 ~ 10, described organic amine can be selected from n-butylamine, ethylenediamine, normal-butyl ammonium bromide and TPAOH one or more.
Preferably, in described step 4, the concentration of acid solution is 0.1-8mol/L, and the liquid-solid ratio of acid solution and pressed powder is 10-300ml/g, after pressed powder mixes with acid solution, and stirring at normal temperature 30min.Described acid solution can be selected from sulfuric acid, hydrochloric acid and nitric acid one or more.
The present invention uses alkali-metal carbonate as alkaline process process alkali used, and adds organic amine, contrasts, have the following advantages with existing method:
(1) alkali treatment use alkali and non-common NaOH, KOH, LiOH; but the carbonate used; the alkalescence of carbonate due to carbanion hydrolysis degree limited and there will not be alkalescence to cross strong and cause the duct of molecular sieve to be occurred by the situation of excess destruction, thus effectively protect the pore passage structure of molecular sieve.
(2) introducing of organic amine can promote on the one hand the carrying out of desilication, forms meso-hole structure quickly, and in the middle of Zeolite synthesis, organic amine, can the microcellular structure of molecular sieves stabilized inside better as conventional template on the other hand.
(3) last pickling not only can reach the effect of the alkali that removing is not cleaned, and can also remove the unformed aluminium because early stage generates after alkaline process desiliconization process, has arrived the effect of dredging duct and increase specific area.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail,
Embodiment one
A method of modifying for preparing gasoline by methanol molecular sieve, comprises the following steps:
Step one, by the Na of 10g molecular sieve and 500ml 0.5mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g n-butylamine, airtight container, at 140 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 500ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 140 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 1.
The present embodiment Activity evaluation is in table one.
Embodiment two
Step one, by the Na of 10g molecular sieve and 500ml 0.5mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g ethylenediamine, airtight container, at 140 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 500ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 140 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 2.
The present embodiment Activity evaluation is in table one.
Embodiment three
Step one, by the Na of 10g molecular sieve and 500ml 0.5mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g TPAOH, airtight container, at 140 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 500ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 140 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 3.
The present embodiment Activity evaluation is in table one.
Embodiment four
Step one, by the K of 10g molecular sieve and 500ml 0.5mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g n-butylamine, airtight container, at 140 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 500ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 140 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 4.
The present embodiment Activity evaluation is in table one.
Embodiment five
A method of modifying for preparing gasoline by methanol molecular sieve, comprises the following steps:
Step one, by the Na of 10g molecular sieve and 500ml 0.5mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g n-butylamine, airtight container, at 140 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the salpeter solution of 500ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 140 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 5.
The present embodiment Activity evaluation is in table one.
Embodiment six
A method of modifying for preparing gasoline by methanol molecular sieve, comprises the following steps:
Step one, by the Na of 10g molecular sieve and 1000ml 0.5mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g n-butylamine, airtight container, at 140 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 1000ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 140 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 6.
The present embodiment Activity evaluation is in table one.
Embodiment seven
A method of modifying for preparing gasoline by methanol molecular sieve, comprises the following steps:
Step one, by the Na of 10g molecular sieve and 500ml 2mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g n-butylamine, airtight container, at 140 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 500ml 2mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 140 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 7.
The present embodiment Activity evaluation is in table one.
Embodiment eight
A method of modifying for preparing gasoline by methanol molecular sieve, comprises the following steps:
Step one, by the Na of 10g molecular sieve and 500ml 0.5mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g n-butylamine, airtight container, at 80 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 500ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 80 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 8.
The present embodiment Activity evaluation is in table one.
Embodiment nine
A method of modifying for preparing gasoline by methanol molecular sieve, comprises the following steps:
Step one, by the Na of 10g molecular sieve and 1000ml 1mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g n-butylamine, airtight container, at 140 DEG C, heat stir process 3h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 500ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 80 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 9.
The present embodiment Activity evaluation is in table one.
Embodiment ten
A method of modifying for preparing gasoline by methanol molecular sieve, comprises the following steps:
Step one, by the K of 10g molecular sieve and 1000ml 2mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 10g n-butylamine, airtight container, at 120 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 800ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 80 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 10.
The present embodiment Activity evaluation is in table one.
Embodiment 11
A method of modifying for preparing gasoline by methanol molecular sieve, comprises the following steps:
Step one, by the Na of 20g molecular sieve and 500ml 0.5mol/L
2cO
3solution mixes, stirring at normal temperature 30min;
Step 2, step one mixture to be proceeded to teflon-lined autoclave, add 30g n-butylamine, airtight container, at 110 DEG C, heat stir process 4h;
Step 3, the mixture of step 2 is cooled to room temperature, vacuum filtration, uses deionized water washing to neutral, 110 DEG C of dried overnight;
Step 4, step 3 gained pressed powder to be mixed with the hydrochloric acid solution of 500ml 0.5mol/L, stirring at normal temperature 30min, be placed in teflon-lined autoclave, at 110 DEG C, heat stir process 4h;
Step 5, the mixture of step 4 is cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve 11.
The present embodiment Activity evaluation is in table one.
The catalytic activity of the molecular sieve catalyst that the above embodiment of the present invention gained is modified measures, and carries out in fixed bed reactors.Modified molecular sieve catalyst pressed powder is sieved, get 40 ~ 60 molecules of interest sieve catalyst particles to mix with quartz sand and load in reactor, use constant-flux pump that methyl alcohol is injected preheater to mix with carrier gas nitrogen, then enter fixed bed reactors to react, reaction condition: reaction temperature 350 DEG C, reaction pressure 2MPa, mass space velocity 2h
-1, after reaction 24h, collect product liquid.By gas chromatograph on-line analysis, calculate the methanol conversion of MTG reaction and the selective of product.
Illustrated by embodiment, the MTG molecular sieve catalyst prepared according to method of modifying of the present invention has the advantages such as catalytic activity is good, preparation technology is simple, with low cost, is a kind of MTG molecular sieve catalyst having very much actual application prospect.
The MTG activity of molecular sieve catalysts evaluation result of each embodiment catalyst of table one
| Methanol conversion (%) | Oil product yield (wt.%) * | |
| Embodiment one | 99.1 | 35.6 |
| Embodiment two | 98.9 | 36.3 |
| Embodiment three | 99.2 | 38.4 |
| Embodiment four | 99.2 | 39.2 |
| Embodiment five | 99.1 | 37.5 |
| Embodiment six | 99 | 39.1 |
| Embodiment seven | 98.8 | 38.4 |
| Embodiment eight | 99.3 | 38.5 |
| Embodiment nine | 99.5 | 38.9 |
| Embodiment ten | 99.1 | 39.2 |
| Embodiment 11 | 99 | 39.1 |
* oil product yield=(methanol quality of oil quality/injection that collection obtains) * 100.
Claims (8)
1., for a modification processing method for the molecular sieve of preparing gasoline by methanol reaction, it is characterized in that, comprise the steps:
Step one, by be used for preparing gasoline by methanol reaction molecular sieve and aqueous slkali mix and blend obtain mixture, wherein said aqueous slkali is selected from Li
2cO
3, Na
2cO
3and K
2cO
3in one or more;
Step 2, mixture step one obtained proceed to teflon-lined autoclave, add organic amine, heat stir process 0.5-8h after sealing at 50-200 DEG C;
Step 3, step 2 is heated after mixture be cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, obtain pressed powder;
Step 4, by step 3 gained pressed powder and acid solution mix and blend, be then placed in teflon-lined autoclave, at 50-200 DEG C, heat stir process 0.5-8h;
Step 5, step 4 is heated after mixture be cooled to room temperature, vacuum filtration, use deionized water washing to neutral, 110 DEG C of dried overnight, are placed in Muffle furnace 400 DEG C of high-temperature calcinations, obtain modified molecular sieve.
2., according to claim 1 for the modification processing method of the molecular sieve of preparing gasoline by methanol reaction, it is characterized in that, in described step one, alkaline concentration is 0.1-8mol/L, and the liquid-solid ratio of aqueous slkali and molecular sieve is 10-300ml/g.
3. according to claim 1 or 2 for the modification processing method of molecular sieve of preparing gasoline by methanol reaction, it is characterized in that, in described step one, after molecular sieve mixes with aqueous slkali, stirring at normal temperature 30min.
4., according to claim 1 for the modification processing method of the molecular sieve of preparing gasoline by methanol reaction, it is characterized in that, in described step 2, the organic amine added and the mass ratio of molecular sieve are 0.1 ~ 10.
5. according to claim 1 or 4 for the modification processing method of molecular sieve of preparing gasoline by methanol reaction, it is characterized in that, in described step 2, described organic amine be selected from n-butylamine, ethylenediamine, normal-butyl ammonium bromide and TPAOH one or more.
6., according to claim 1 for the modification processing method of the molecular sieve of preparing gasoline by methanol reaction, it is characterized in that, in described step 4, the concentration of acid solution is 0.1-8mol/L, and the liquid-solid ratio of acid solution and pressed powder is 10-300ml/g.
7. according to claim 1 or 6 for the modification processing method of molecular sieve of preparing gasoline by methanol reaction, it is characterized in that, in described step 4, after pressed powder mixes with acid solution, stirring at normal temperature 30min.
8., according to claim 7 for the modification processing method of molecular sieve of preparing gasoline by methanol reaction, it is characterized in that, described acid solution be selected from sulfuric acid, hydrochloric acid and nitric acid one or more.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629766A (en) * | 2015-10-30 | 2017-05-10 | 中国科学院上海高等研究院 | Hierarchical porous molecular sieve and alkali treatment solid-phase synthetic method thereof |
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| US5573990A (en) * | 1992-05-03 | 1996-11-12 | Dalian Institute Of Chemical Physics | Process for the conversion of methanol to light olefins and catalyst for such process |
| CN103433067A (en) * | 2013-09-09 | 2013-12-11 | 中国科学院上海高等研究院 | Catalyst for preparing gasoline from methyl alcohol as well as preparation and application of catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5573990A (en) * | 1992-05-03 | 1996-11-12 | Dalian Institute Of Chemical Physics | Process for the conversion of methanol to light olefins and catalyst for such process |
| CN103433067A (en) * | 2013-09-09 | 2013-12-11 | 中国科学院上海高等研究院 | Catalyst for preparing gasoline from methyl alcohol as well as preparation and application of catalyst |
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| Title |
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| CN106629766A (en) * | 2015-10-30 | 2017-05-10 | 中国科学院上海高等研究院 | Hierarchical porous molecular sieve and alkali treatment solid-phase synthetic method thereof |
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