CN101844087B - Preparation method of propylene catalyst prepared by methanol transformation - Google Patents
Preparation method of propylene catalyst prepared by methanol transformation Download PDFInfo
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- CN101844087B CN101844087B CN2010102057947A CN201010205794A CN101844087B CN 101844087 B CN101844087 B CN 101844087B CN 2010102057947 A CN2010102057947 A CN 2010102057947A CN 201010205794 A CN201010205794 A CN 201010205794A CN 101844087 B CN101844087 B CN 101844087B
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Abstract
The invention discloses a preparation method of a propylene catalyst prepared by methanol transformation, which comprises the following steps of: adding hydrogen type ZSM-5 molecular sieve powder with the silicon-aluminum molar ratio of 50 to 250 into water to obtain uniform slurry; adding a phosphoric acid solution into the slurry; adding the nitrate or the acetate of magnesium or cerium into the slurry, wherein the mass ratio of the additive to the hydrogen type ZSM-5 molecular sieve powder is 0.2 to 5:100; and adding the nitrate, the carbonate or the acetate of sodium or potassium into the slurry, putting the slurry into a water bath with constant temperature of 60 to 90 DEG C, stirring for 3 to 5 hours and calcining at the temperature of 400 to 550 DEG C for 4 to 8 hours to prepare the required catalyst after drying at the temperature of 100 to 120 DEG C and grinding into powder, wherein the mass ratio of the additive to the hydrogen type ZSM-5 molecular sieve powder is 0.01 to 3:100. The catalyst prepared by the method has high propylene selectivity and favorable thermal stability.
Description
Technical field
The present invention relates to a kind of preparation method of propylene catalyst from methanol conversion.
Background technology
Propylene is the petrochemical industry basic material that most important and consumption is only second to ethene beyond the ethene, can be in order to produce multiple important Organic Chemicals, like acrylonitrile, epoxychloropropane, expoxy propane, isopropyl alcohol, glycerine, acetone, acrylate etc.; Also can directly synthesize polypropylene, EP rubbers, acrylic fibers, polypropylene fibre etc.; It in petroleum refining industry the raw material of producing polymer gasoline.
Along with to the increasing rapidly of the demand of propylene and derivative thereof, the demand of propylene is also risen year by year.The crude oil that traditional production of propylene technological requirement is a large amount of or the supply of liquefied petroleum gas; The rising significantly and the future petroleum energy of whole world oil price face exhaustion, press for the energy crisis that new energy substitution product of exploitation and new process cause with the shortage of solution future petroleum.By methyl alcohol is that catalytic material is produced the novel process that the propylene technology is hopeful to replace petroleum path most.Preparing propylene from methanol Study on Technology, exploitation and industrialization become one of important focus of domestic and international technological development in recent years, and the key of this technology is the development of high performance catalyst.
At present, the catalyst that preparing propylene by methanol transformation adopted mainly contains aluminum phosphate series molecular sieve and alumina silicate series molecular sieve.A kind of aluminum phosphate series molecular sieve (SAPO-n) is disclosed in U.S. Pat 4440871; Wherein aluminium phosphate molecular sieve SAPO-34 produces alkene to methyl alcohol has certain catalytic performance, but yield of ethene reaches 53.8% in its product, and propene yield is merely 29.1%; Simultaneously; SAPO series molecular sieve catalyst aperture is little, is prone to coking, so methanol conversion is produced less employing in the propylene technology.
U.S. Mobil company prepares in the gasoline process and finds at research methyl alcohol, can realize the production of methyl alcohol to light alkene through al silicate molecular sieve catalyst ZSM-5 being modified and changing reaction condition.The propylene selectivity of ZSM-5 molecular sieve catalyst in the methyl alcohol reaction is better than SAP0-34, and has anti-coking performance and hydrothermal stability preferably, produces in the propylene technology in methanol conversion at present and extensively adopts.
Because the aperture of aluminum phosphate series molecular sieve and alumina silicate series molecular sieve is less, can limit the generation of big molecular product, thereby low-carbon alkene (ethene, propylene and butylene) selectivity is improved in the product, realizes the production of methyl alcohol to light alkene.Yet because above-mentioned two types of selection of catalysts property are to be achieved through the aperture is little; Its result increases low-carbon alkene such as ethene and propylene the time often; Can not reach and improve the requirement that propylene optionally reduces ethylene selectivity simultaneously, can not satisfy the needs of preparing propylene by methanol transformation effectively.
Summary of the invention
The objective of the invention is to overcome that methanol conversion prepares the propylene catalyst deficiency not high to the propylene selectivity in the prior art, a kind of preparation method of propylene catalyst from methanol conversion is provided.The catalyst that this method is produced has high propylene selectivity and good heat endurance.
For realizing above-mentioned purpose, the technical solution adopted for the present invention to solve the technical problems is:
A kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 50～250 Hydrogen ZSM-5 molecular sieve powder adds in the entry, obtain homogeneous slurry silica alumina ratio;
B, in the slurries that steps A obtains, add phosphoric acid solution, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 1～6:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add the nitrate or the acetate of magnesium or cerium, the mass ratio of this additive and Hydrogen ZSM-5 molecular sieve powder is 0.2～5:100;
D, in the slurries that step C obtains, add nitrate, carbonate or the acetate of sodium or potassium; The mass ratio of this additive and Hydrogen ZSM-5 molecular sieve powder is 0.01～3:100; Slurries place water bath with thermostatic control under 60～90 ℃ of temperature, to stir 3～5 hours; Dry and pulverize lastly under 100～120 ℃ of temperature, 400～550 ℃ of roasting temperatures 4～8 hours, make required catalyst.
As optimal way, the silica alumina ratio of Hydrogen ZSM-5 molecular sieve is 70～200 in the said steps A; Further preferred, the silica alumina ratio of Hydrogen ZSM-5 molecular sieve is 90～150 in the said steps A; Most preferably, the silica alumina ratio of Hydrogen ZSM-5 molecular sieve is 100 in the said steps A.
As optimal way, in said step B, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in the phosphoric acid solution; In said step C, the mass ratio of additive and Hydrogen ZSM-5 molecular sieve powder is 0.5～2:100; In said step D, the mass ratio of additive and Hydrogen ZSM-5 molecular sieve powder is 0.05～1:100.
As optimal way, roasting is carried out in Muffle furnace in the said steps A.
The present invention introduces phosphorus and magnesium or phosphorus and cerium, can partly cover strong acidic site, reduces the acidic site density of molecular sieve, effectively suppresses the generation of hydrogen migration, thereby improves the anti-coking performance of molecular sieve; And phosphorus can also effectively suppress the dealuminzation inactivation of molecular sieve, improves its heat endurance.On the basis of adding phosphorus and magnesium or phosphorus and cerium, add nitrate, carbonate or the acetate of sodium or potassium simultaneously, Hydrogen ZSM-5 molecular sieve is carried out modification, obtained composite catalyst.The preparing propylene by methanol transformation reaction belongs to the exothermic reaction of hydrocarbon under the acid catalysis; Its reactivity worth receives the acid catalysis Effect on Performance, and the present invention introduces sodium or potassium, can adjust acid structure; Help the carrying out that react, thereby optionally reduce ethylene selectivity simultaneously improving propylene.
Beneficial effect of the present invention is: it is low that the present invention has mainly solved the purpose product propene yield that exists in the prior art; Problems such as the poor heat stability of catalyst; And method for preparing catalyst technology is simple, because the interpolation of sodium or potassium has reduced the Preparation of catalysts cost to a certain extent.Adopt technical scheme of the present invention, the propylene selectivity reaches as high as 48%, and the methyl alcohol conversion per pass still can keep having obtained the good technical effect more than 99% after 280 hours in reaction.
The specific embodiment
Disclosed arbitrary characteristic in this specification is only if special narration all can be replaced by other equivalences or the alternative features with similar purpose.That is, only if special narration, each characteristic is an example in a series of equivalences or the similar characteristics.
Fixed bed reactors are adopted in the activity of such catalysts evaluation among the present invention, are that raw material, water are that diluent, methanol quality air speed are 1 hour with methyl alcohol
-1, water/methanol quality is than being 2:1, methanol conversion preparing dimethy ether catalytic reaction temperature is 290 ℃, catalysis system propylene reaction temperature is 480 ℃, normal pressure.
Comparative example 1: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 50～250 Hydrogen ZSM-5 molecular sieve powder adds in the entry, obtain homogeneous slurry silica alumina ratio;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 0.5 gram magnesium nitrate; Slurries place water bath with thermostatic control under 60～90 ℃ of temperature, to stir 3～5 hours then, and are dry and pulverize lastly under 120 ℃ of temperature, 550 ℃ of roasting temperatures 8 hours, make required catalyst.Table 1 is seen in this activity of such catalysts evaluation.
Embodiment 1: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 50～250 Hydrogen ZSM-5 molecular sieve powder adds in the entry, obtain homogeneous slurry silica alumina ratio;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 0.5 gram magnesium nitrate, stir;
D, in the slurries that step C obtains, add 0.05 gram potassium acetate; Stir, slurries place water bath with thermostatic control under 90 ℃ of temperature, to stir 3 hours, and are dry and pulverize last under 120 ℃ of temperature; 550 ℃ of roasting temperatures 8 hours, make required catalyst.Table 1 is seen in this activity of such catalysts evaluation.
Embodiment 2: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 100 Hydrogen ZSM-5 molecular sieve powder is dissolved in the water, obtain homogeneous slurry 200 gram silica alumina ratios;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 4 gram magnesium nitrates, stir;
D, in the slurries that step C obtains, add 0.1 gram potassium acetate, slurries place water bath with thermostatic control under 60 ℃ of temperature, to stir 5 hours, and drying and pulverize lastly under 120 ℃ of temperature 550 ℃ of roasting temperatures 8 hours, makes required catalyst.Table 1 is seen in this activity of such catalysts evaluation.
Embodiment 3: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 70 Hydrogen ZSM-5 molecular sieve powder adds in the entry, obtain homogeneous slurry silica alumina ratio;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 0.5 gram cerous acetate;
D, in the slurries that step C obtains, add 0.05 gram potassium acetate, slurries place water bath with thermostatic control under 90 ℃ of temperature, to stir 3 hours, and drying and pulverize lastly under 100 ℃ of temperature 550 ℃ of roasting temperatures 8 hours, makes required catalyst.Table 1 is seen in this activity of such catalysts evaluation.
Embodiment 4: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 90 Hydrogen ZSM-5 molecular sieve powder is dissolved in the water, obtain homogeneous slurry 200 gram silica alumina ratios;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 1 gram magnesium nitrate;
D, in the slurries that step C obtains, add 0.1 gram potash, slurries place water bath with thermostatic control under 90 ℃ of temperature, to stir 3 hours, drying and pulverize lastly under 120 ℃ of temperature, and 400 ℃ of roasting temperatures are 8 hours in Muffle furnace, make required catalyst.Table 1 is seen in this activity of such catalysts evaluation.
Embodiment 5: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 150 Hydrogen ZSM-5 molecular sieve powder is dissolved in the water, obtain homogeneous slurry 300 gram silica alumina ratios;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 1.5 gram magnesium nitrates;
D, in the slurries that step C obtains, add 0.3 gram sodium nitrate, slurries place water bath with thermostatic control under 90 ℃ of temperature, to stir 3 hours, and drying and pulverize lastly under 120 ℃ of temperature 550 ℃ of roasting temperatures 8 hours, makes required catalyst.Table 1 is seen in this activity of such catalysts evaluation.
Embodiment 6: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 200 Hydrogen ZSM-5 molecular sieve powder is dissolved in the water, obtain homogeneous slurry 300 gram silica alumina ratios;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 1:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 1.5 gram magnesium nitrates;
D, in the slurries that step C obtains, add 0.15 gram potassium acetate, slurries place water bath with thermostatic control under 90 ℃ of temperature, to stir 3 hours, and drying and pulverize lastly under 120 ℃ of temperature 550 ℃ of roasting temperatures 8 hours, makes required catalyst.Table 1 is seen in this activity of such catalysts evaluation.
The activity rating table of table 1 propylene catalyst from methanol conversion
| Title | Methanol conversion % | Propylene selectivity % | Life-span/h |
| Comparative example 1 | 99.5 | 36.7 | 201 |
| Embodiment 1 | 99.9 | 40.3 | 231 |
| Embodiment 2 | 99.7 | 48.2 | 282 |
| Embodiment 3 | 99.9 | 34.6 | 220 |
| Embodiment 4 | 99.8 | 37.2 | 207 |
| Embodiment 5 | 99.4 | 45.3 | 175 |
| Embodiment 6 | 99.7 | 35.4 | 205 |
Catalyst life index in the table 1 is that methanol conversion is greater than 99%.
Visible by last table, technical scheme of the present invention is superior to comparative example in the data aspect methanol conversion, propylene selectivity and the catalyst life, has high propylene selectivity.
Embodiment 7: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 50 Hydrogen ZSM-5 molecular sieve powder is dissolved in the water, obtain homogeneous slurry 100 gram silica alumina ratios;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 0.5 gram magnesium nitrate;
D, in the slurries that step C obtains, add 0.05 gram potassium acetate, slurries place water bath with thermostatic control under 90 ℃ of temperature, to stir 3 hours, and drying and pulverize lastly under 120 ℃ of temperature 550 ℃ of roasting temperatures 8 hours, makes required catalyst.
Embodiment 8: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 250 Hydrogen ZSM-5 molecular sieve powder is dissolved in the low amounts of water, make molecular sieve powder be submerged, and stir, obtain homogeneous slurry 200 gram silica alumina ratios;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 0.4 gram magnesium nitrate;
D, in the slurries that step C obtains, add 0.02 gram potassium acetate, slurries place water bath with thermostatic control under 90 ℃ of temperature, to stir 3 hours, and drying and pulverize lastly under 120 ℃ of temperature 550 ℃ of roasting temperatures 8 hours, makes required catalyst.
Embodiment 9: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 80 Hydrogen ZSM-5 molecular sieve powder is dissolved in the low amounts of water, make molecular sieve powder be submerged, and stir, obtain homogeneous slurry 100 gram silica alumina ratios;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 1:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 0.2 gram magnesium nitrate;
D, in the slurries that step C obtains, add 0.01 gram potash; Slurries place water bath with thermostatic control under 90 ℃ of temperature, to stir 3 hours; Dry and pulverize lastly under 120 ℃ of temperature, 400 ℃ of roasting temperatures are 8 hours in Muffle furnace, make required catalyst.Table 1 is seen in this activity of such catalysts evaluation.
Embodiment 10: a kind of preparation method of propylene catalyst from methanol conversion may further comprise the steps:
A, be that 150 Hydrogen ZSM-5 molecular sieve powder is dissolved in the water, obtain homogeneous slurry 200 gram silica alumina ratios;
B, in the slurries that steps A obtains, add the phosphoric acid solution of concentration 85%, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 6:100 in this phosphoric acid solution;
C, in the slurries that step B obtains, add 10 gram magnesium nitrates;
D, in the slurries that step C obtains, add 6 gram sodium nitrate, slurries place water bath with thermostatic control under 90 ℃ of temperature, to stir 3 hours, and drying and pulverize lastly under 120 ℃ of temperature 550 ℃ of roasting temperatures 8 hours, makes required catalyst.Table 1 is seen in this activity of such catalysts evaluation.
The present invention is not limited to the aforesaid specific embodiment.The present invention expands to any new feature or any new combination that discloses in this manual, and the arbitrary new method that discloses or step or any new combination of process.
Claims (5)
1. the preparation method of a propylene catalyst from methanol conversion is characterized in that may further comprise the steps:
A, be that 50～250 Hydrogen ZSM-5 molecular sieve powder adds in the entry, obtain homogeneous slurry silica alumina ratio;
B, in the slurries that steps A obtains, add phosphoric acid solution, phosphorus pentoxide content and Hydrogen ZSM-5 in this phosphoric acid solution
The mass ratio of molecular sieve powder is l～6:100;
C, in the slurries that step B obtains, add the nitrate or the acetate of magnesium or cerium, the mass ratio of this additive and Hydrogen ZSM-5 molecular sieve powder is 0.2～5:100;
D, in the slurries that step C obtains, add nitrate, carbonate or the acetate of sodium or potassium, this additive and Hydrogen
The mass ratio of ZSM-5 molecular sieve powder is 0.01～3:100, and slurries place water bath with thermostatic control under 60～90 ℃ of temperature, to stir
3～5 hours, under 100-120 ℃ of temperature dry and pulverize last, at 400～550 ℃ of roasting temperatures 4～8
Hour, make required catalyst.
2. the preparation method of a kind of propylene catalyst from methanol conversion as claimed in claim 1 is characterized in that: the said step
Roasting is carried out in Muffle furnace among the rapid D.
3. the preparation method of a kind of propylene catalyst from methanol conversion as claimed in claim 1 is characterized in that: said
Among the step B, the mass ratio of phosphorus pentoxide content and Hydrogen ZSM-5 molecular sieve powder is 2:100 in the phosphoric acid solution.
4. the preparation method of a kind of propylene catalyst from methanol conversion as claimed in claim 1 is characterized in that: said
Among the step C, the mass ratio of additive and Hydrogen ZSM-5 molecular sieve powder is 0.5～2:100.
5. the preparation method of a kind of propylene catalyst from methanol conversion as claimed in claim 1 is characterized in that: said
Among the step D, the mass ratio of additive and Hydrogen ZSM-5 molecular sieve powder is 0.05～l:100.
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| CN102658212B (en) * | 2010-10-26 | 2014-03-19 | 安徽淮化股份有限公司 | Method for grinding and mixing coal-to-olefin catalyst slurry |
| CN102527426A (en) * | 2011-12-15 | 2012-07-04 | 西南化工研究设计院 | Preparation method for catalyst for preparing ethylene by dehydrating ethanol |
| CN102675026B (en) * | 2012-05-04 | 2015-11-18 | 山东京博控股股份有限公司 | A kind of two-part preparation technology of propylene |
| CN104069888A (en) * | 2013-03-29 | 2014-10-01 | 上海碧科清洁能源技术有限公司 | Modified ZSM-5 molecular sieve catalyst and preparation method and application thereof |
| CN105712377A (en) * | 2014-12-01 | 2016-06-29 | 中国石油天然气股份有限公司 | Mesoporous ZSM-5 molecular sieve, and preparation method thereof |
| CN114308110B (en) * | 2021-11-24 | 2024-04-05 | 新疆恒有能源科技股份有限公司 | Preparation method of molecular sieve catalyst for preparing olefin by fluidized catalytic cracking of methanol |
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| CN101239875A (en) * | 2007-02-07 | 2008-08-13 | 中国石油化工股份有限公司 | Method for preparing propylene from methanol |
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| CN101130469B (en) * | 2006-08-23 | 2011-04-13 | 中国科学院大连化学物理研究所 | Method for recovering reactivation heat in process of preparing low carbon olefinic hydrocarbon with methanol |
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| CN101176849A (en) * | 2006-11-07 | 2008-05-14 | 中国科学院大连化学物理研究所 | Catalyzer for preparing propylene from methanol or dimethyl ether in high selectivity and preparation method thereof |
| CN101239875A (en) * | 2007-02-07 | 2008-08-13 | 中国石油化工股份有限公司 | Method for preparing propylene from methanol |
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