CN101172917B - Method for producing ethylene, propylene - Google Patents

Method for producing ethylene, propylene Download PDF

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Publication number
CN101172917B
CN101172917B CN2006101178632A CN200610117863A CN101172917B CN 101172917 B CN101172917 B CN 101172917B CN 2006101178632 A CN2006101178632 A CN 2006101178632A CN 200610117863 A CN200610117863 A CN 200610117863A CN 101172917 B CN101172917 B CN 101172917B
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propylene
reaction
methyl alcohol
ethene
dme
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CN101172917A (en
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杨为民
刘俊涛
钟思青
朱志焱
刘红星
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/40—Ethylene production

Abstract

The invention relates to a preparation method of ethylene and propylene, and mainly solves the technical problems of short service time of the catalyst and large energy consumption of the prior art. The invention takes methyl alcohol and dimethyl ether as raw materials and ethanol as thinner, wherein, the weight proportion of the methyl alcohol and the dimethyl ether is 0 to 100:100 to 0; and theweight proportion of the methyl alcohol and the dimethyl ether and the ethanol is larger than 0 to 6: 1. The raw materials is contacted with crystalloid sillico aluminate catalyst 2 which has the molratio of silicate to aluminum (Sio2AL2O3) of at least 10 to generate a reaction effluent which has the ethylene and the propylene at the reaction temperature of 400 to 580 DEG C, the reaction weight space velocity of 0.1 to 20 hours<-1> and the reaction pressure of 0.01 to 2 MPa. The reaction effluent is separated to obtain the product of the ethylene and the propylene. The invention preferably solves the technical problems mentioned above, and the invention can be applied to the industrial production of the ethylene and the propylene.

Description

Produce the method for ethene and propylene
Technical field
The present invention relates to a kind of method of producing ethene and propylene, is the methyl alcohol of thinner and the method that dimethyl ether catalysis transforms production ethene and propylene about ethanol particularly.
Background technology
Petrochemical complex is a mainstay industry important in the national economy, for industry, agricultural, departments such as traffic and national defence provide a large amount of industrial chemicals, is one of related and branch of industry that drive property is stronger in the national economy.Propylene and ethene then are to constitute modern petrochemical complex of paramount importance two big basic materials.
Propylene is mainly used in produces polypropylene, isopropyl benzene, oxo-alcohols, vinyl cyanide, propylene oxide, vinylformic acid, Virahol etc., and wherein polypropylene accounts for the over half of world's propylene demand.At present, 67% propylene is produced the byproduct of ethene from steam cracking in the world, and 30% produces the byproduct of vapour, diesel oil from refinery catalytic cracking (FCC), and a small amount of (about 3%) is obtained by dehydrogenating propane and ethene-butylene metathesis reaction.Estimate that following propylene demand growth speed is faster than supply.
Higher in view of the growth rate of demand of propylene, and traditional production model presents the pressure of " supply falls short of demand ", and therefore replenishing the propylene demand need be by means of other various propylene enhancing new technology.
All the time; coal or Sweet natural gas preparing synthetic gas, synthesising gas systeming carbinol and alkene isolation technique have had the mass-producing mature experience; but the process by methanol to olefins is breakpoint and the difficult point of synthetic gas to this industrial chain of alkene, and this solution of key technology can be for providing a new raw material route by non-oil resource production basic organic ethene, propylene.Especially in the last few years, it is high that the demand of ethene and propylene continues, and under the deficient day by day situation of petroleum resources.How to hew out a non-oil resource and produce the Coal Chemical Industry variation route of propylene, for greatly alleviating China's oil situation in short supply, promote the great-leap-forward development of the heavy chemical industry of China and the structural adjustment of raw material route, have important strategic meaning and society, economic benefit.
Document CN1166478A, disclose a kind of method of being produced low-carbon alkenes such as ethene, propylene by methyl alcohol or dme, this method is catalyzer with the aluminium phosphate molecular sieve, adopts the ciculation fluidized formula processing method of upstriker dense bed, in 500～570 ℃ of preferred temperature of reaction, air speed 2～6 hours -1And under 0.01～0.05MPa condition, make methyl alcohol or dme cracking produce low-carbon alkenes such as ethene, propylene.This method one side, temperature is higher, and the purpose product selectivity is low, adopts fluidization to have cost of investment and the higher technical disadvantages of running cost simultaneously.
Document CN1356299A discloses a kind of processing method and system thereof that produces low-carbon alkene by methyl alcohol or dme.This process using silicoaluminophosphamolecular molecular sieves (SAPO-34) is as catalyzer, utilize the ultrashort contact reactor of gas-solid cocurrent flow descending formula fluidized-bed, catalyzer contacts in the ultrashort contact reactor of gas-solid cocurrent flow descending formula fluidized-bed with raw material, the reactant flow direction is descending; Catalyzer and reaction product go out to enter the gas-solid quick disconnector that is arranged on this reactor lower part behind the reactor and carry out sharp separation; Isolated catalyzer enters charcoal regeneration in the revivifier, and catalyzer is cyclic regeneration in system, and reaction cycle is carried out.This technology dme or conversion of methanol are greater than 98%.But this method exists equally, and the ethylene, propylene selectivity is low, cost of investment and the higher technical disadvantages of running cost.
Document CN1704390A discloses a kind of method of methanol conversion system alkene, this method employing Zn-SAPO-34 molecular sieve and binding agent are as the catalyzer of methanol conversion system alkene, 300～500 ℃ of temperature of reaction, reaction pressure is a normal pressure, and the methyl alcohol weight space velocity is 1.0～10 hours -1, water/methyl alcohol weight ratio is that reaction generates low-carbon alkene under 0～5 condition.This method catalyst life is short, needs by fluidized-bed process the flow process complexity.
Problems such as the technology of above-mentioned bibliographical information mainly exists life of catalyst shorter, needs to adopt fluidization, and investment is high, and energy consumption is big.
Technical problem to be solved by this invention is that to overcome the life of catalyst that exists in the technical literature in the past shorter, and investment is high, and the problem that energy consumption is big provides a kind of new production ethene and the method for propylene.It is good that this method has a catalyst stability, energy effective utilization rate height, the advantage that propene yield is high.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method of producing ethene and propylene, with methyl alcohol, dme and ethanol is raw material, wherein the weight ratio of methyl alcohol and dme is 0～100: 100～0, methyl alcohol and dme weight and ethanol weight ratio are 0.5～6: 1, in temperature of reaction is 400～580 ℃, and the reaction weight space velocity is 0.1～20 hour -1, reaction pressure is under 0.01～2MPa condition, raw material contacts with the crystal aluminosilicate catalyzer, generates the reaction effluent that contains ethene, propylene, obtains ethene, propylene product through separation; Wherein, the crystal aluminosilicate catalyzer is for being selected from silica alumina ratio SiO 2/ Al 2O 3Be 40～400 ZSM-5 molecular sieve, silica alumina ratio 8iO 2/ Al 2O 3Be 20～600 beta-molecular sieve or silica alumina ratio SiO 2/ Al 2O 3Be at least a in 20～600 the mordenite.
The temperature of reaction preferable range is 450～510 ℃ in the technique scheme, and reaction weight space velocity preferable range is 0.5～10 hour -1, the reaction pressure preferable range is 0.05～1MPa; Methyl alcohol and dme weight and ethanol weight ratio preferable range are 0.5～3: 1.
Adopting ethanol among the present invention is thinner, has realized the catalytic cracking ethene of methyl alcohol and dme and the reaction of propylene.Because it is strong exothermic process that methyl alcohol and dme are produced low-carbon alkene, for adopting fixed-bed process, the concentrated heat release of dehydration can cause the higher temperature rise of beds, especially the temperature of catalyst active center may exceed catalyzer apparent temperature tens degree even more than 100 ℃, and too high local temperature rise is very fatal to the influence of catalyst life, especially can aggravate catalyzer coking inactivation greatly, shorten stable period.Simultaneously, concentrate strong heat release also to bring big difficulty for reactor design and engineering amplification, and the subsidiary much energy consumption that increases.And the producing ethylene from dehydration of ethanol process is a strong endothermic reaction, and reaction process has higher adiabatic temperature drop.Among the present invention fully in conjunction with ethanol dehydration and methyl alcohol and dme system olefine reaction characteristics and essence; be reflected in the same reactor two and carry out; rational proportion by material quantity; make endothermic heat of reaction, thermal discharge be in equilibrium state; avoided ascending to heaven of reaction bed temperature; effectively protect catalyzer, prolonged catalyst life, improved stability.Simultaneously, because the caloric receptivity and the complementation of thermal discharge original position of two reactions make heat of reaction just obtain effective utilization in reaction process.The synergy of the catalytic cracking ethene of ethanol dehydration reaction process and methyl alcohol and dme, propylene reaction also has remarkable promoter action to the yield that improves ethene and propylene.
Adopt technical scheme of the present invention, at crystal aluminosilicate ZSM-5 molecular sieve silica alumina ratio SiO 2/ Al 2O 3Be 40～400, temperature of reaction is 450～510 ℃, the reaction weight space velocity is 0.5～10 hour-1, reaction pressure is 0.05～1MPa, methyl alcohol and dme raw material and ethanol weight ratio are under 0.5～3: 1 the condition, the propene yield rate can reach 45%, and catalyst life can surpass 450 hours, has obtained better technical effect.
The present invention is further elaborated below by embodiment.
Embodiment
[embodiment 1～5]
According to silica alumina ratio SiO 2/ Al 2O 3Be that 100 proportional arrangement is siliceous, the slip of aluminium, template and water, stirred 24 hours under the room temperature.Crystallization 40～100 hours under 110～230 ℃ temperature is then washed crystallization liquid afterwards, is promptly obtained the ZSM-5 molecular sieve after the oven dry, roasting.After the ZSM-5 molecular sieve adding 60 gram silica gel mixing with 100 grams, extrusion moulding, and, make anti-required silica alumina ratio SiO after 530 ℃ of roastings 200 ℃ of oven dry 2/ Al 2O 3It is 100 ZSM-5 type catalyzer.
It is 18 millimeters fixed-bed reactor that the ZSM-5 molecular sieve catalyst that makes 3 grams are put into internal diameter, logical nitrogen is cooled to temperature of reaction 550 ℃ of activation after 2 hours before the experiment, dme and methyl alcohol and ethanol weight ratio are 0: 5: 1 in the raw material that uses in the experiment, in temperature of reaction is 480 ℃, under gauge pressure reaction pressure 0.02MPa condition, the result such as the table 1 that react under the different air speed conditions of methyl alcohol:
The different air speed reaction results of table 1
Numbering 1 2 3 4 5
Air speed, hour -1 1.13 2.74 3.81 4.93 6.63
Yield of ethene, % 20.15 19.33 17.76 15.81 14.63
Propene yield, % 40.88 42.57 44.59 45.84 47.45
Methanol conversion, % 100 100 99.87 99.35 98.93
Ethanol conversion, % 100 100 100 99.87 99.35
[embodiment 6～11]
According to each step and the operational condition of embodiment 1, just change: the silica alumina ratio SiO of ZSM-5 molecular sieve catalyst 2/ Al 2O 3Be 200.Dme and methyl alcohol and ethanol weight ratio are 0: 5: 1 in the raw material that uses in the experiment, are 0.8 hour at the methyl alcohol weight space velocity -1, under gauge pressure reaction pressure 0.05MPa condition, the result such as the table 2 of differential responses temperature:
The result of table 2 differential responses temperature
Numbering 6 7 8 9 10 11
Temperature, ℃ 559 530 478 449 429 404
Yield of ethene, % 27.99 25.77 22.03 20.09 18.01 18.05
Propene yield, % 41.47 43.38 45.15 42.66 39.99 37.39
Methanol conversion, % 100 100 100 99.87 97.53 91.21
Ethanol conversion, % 100 100 100 100 99.70 99.50
[embodiment 12]
According to each step and the operational condition of embodiment 1, just change: the silica alumina ratio SiO of ZSM-5 molecular sieve catalyst 2/ Al 2O 3Be 400.Methyl alcohol and dme and ethanol weight ratio are 2: 2: 1 in the raw material that uses in the experiment, at methyl alcohol and dme weight space velocity is 10 hours-1, in gauge pressure reaction pressure 0.5MPa, under 550 ℃ of conditions of temperature, yield of ethene is 24.73%, propene yield 44.5%, methyl alcohol and dme total conversion rate are 100%, ethanol conversion is 100%.
[embodiment 13]
According to each step and the operational condition of embodiment 1, just change: the silica alumina ratio SiO of ZSM-5 molecular sieve catalyst 2/ Al 2O 3Be 50.Methyl alcohol and dme and ethanol weight ratio are 6: 3: 2 in the raw material that uses in the experiment, are 18 hours at methyl alcohol and dme weight space velocity -1, in gauge pressure reaction pressure 1.5MPa, under 580 ℃ of conditions of temperature, yield of ethene is 24.18%, propene yield 43.41%, and material benzenemethanol and dme total conversion rate are 100%, ethanol conversion is 100%.
[embodiment 14]
According to each step and the operational condition of embodiment 1, just change: catalyzer is silica alumina ratio SiO 2/ Al 2O 3It is 300 β zeolite.Methyl alcohol and dme and ethanol weight ratio are 1: 7: 4 in the raw material that uses in the experiment, at methyl alcohol and dme weight space velocity is 0.5 hour-1, in gauge pressure reaction pressure 0.1MPa, under 450 ℃ of conditions of temperature, yield of ethene is 37.21%, propene yield 36.87%, material benzenemethanol and dme total conversion rate are 98.96%, ethanol conversion is 100%.
[embodiment 15]
According to each step and the operational condition of embodiment 1, just change: catalyzer is silica alumina ratio SiO 2/ Al 2O 3It is 150 mordenite.Methyl alcohol and dme and ethanol weight ratio are 1: 4: 1.5 in the raw material that uses in the experiment, are 0.8 hour at methyl alcohol and dme weight space velocity -1, in gauge pressure reaction pressure 0MPa, under 480 ℃ of conditions of temperature, yield of ethene is 27.22%, propene yield 39.95%, and material benzenemethanol and dme total conversion rate are 100%, ethanol conversion is 100%.
[embodiment 16]
According to each step and the operational condition of embodiment 1, just change: catalyzer is silica alumina ratio SiO 2/ Al 2O 3It is 150 mordenite.Methyl alcohol and dme and ethanol weight ratio are 1: 0: 1 in the raw material that uses in the experiment, are 3.1 hours at the methyl alcohol weight space velocity -1, in gauge pressure reaction pressure 0MPa, under 500 ℃ of conditions of temperature, yield of ethene is 29.22%, and propene yield 40.35%, methanol conversion are 100%, and ethanol conversion is 100%.
[embodiment 13]
According to each step and the operational condition of embodiment 1, just change: the silica alumina ratio SiO of ZSM-5 molecular sieve catalyst 2/ Al 2O 3Be 160.Methyl alcohol and ethanol weight ratio are 6: 0.2 in the raw material that uses in the experiment, are 1.0 hours at the methyl alcohol weight space velocity -1, in gauge pressure reaction pressure 0.2MPa, under 480 ℃ of conditions of temperature, changing ethanol conversion in time is 100%, yield of ethene, propene yield and methanol conversion reaction result are as shown in table 3:
Table 3 is the reacting condition result in time
Reaction times, hour Yield of ethene Propene yield Methanol conversion
1.27 18.61 44.78 98.95
20.55 18.69 44.72 99.08
70.78 18.92 45.14 99.26
92.03 18.76 45.17 99.35
120.28 18.73 45.11 99.05
140.53 19.01 44.91 99.30
180.82 18.73 45.55 99.29
Reaction times, hour Yield of ethene Propene yield Methanol conversion
203.08 18.96 45.1 100
225.5 18.38 45.33 99.32
267.1 18.15 45.8 99.44
290.9 18.50 45.17 99.28
310.42 17.97 45.45 100
340.68 18.32 44.68 99.47
360.98 18.85 44.73 99.69
380.25 19.45 45.82 100
400.57 18.98 45.67 99.13
416.85 18.37 44.67 99.97
432.18 17.19 44.21 98.83
442.47 17.74 43.65 98.61
454.05 17.61 42.45 97.03
465.07 17.48 42.28 96.84
480.1 17.54 42.22 95.80
490.05 16.75 40.82 95.42
500.1 14.38 36.63 95.17
510.5 12.47 34.42 94.09
535.93 9.38 32.29 92.41

Claims (3)

1. method of producing ethene and propylene, with methyl alcohol, dme and ethanol is raw material, wherein the weight ratio of methyl alcohol and dme is 0～100: 100～0, methyl alcohol and dme weight and ethanol weight ratio are 0.5～6: 1, in temperature of reaction is 400～580 ℃, and the reaction weight space velocity is 0.1～20 hour -1, reaction pressure is under 0.01～2MPa condition, raw material contacts with the crystal aluminosilicate catalyzer, generates the reaction effluent that contains ethene, propylene, obtains ethene, propylene product through separation; Wherein, the crystal aluminosilicate catalyzer is for being selected from silica alumina ratio SiO 2/ Al 2O 3Be 40～400 ZSM-5 molecular sieve, silica alumina ratio SiO 2/ Al 2O 3Be 20～600 beta-molecular sieve or silica alumina ratio SiO 2/ Al 2O 3Be at least a in 20～600 the mordenite.
2. according to the method for described production ethene of claim 1 and propylene, it is characterized in that temperature of reaction is 450～510 ℃, the reaction weight space velocity is 0.5～10 hour -1, reaction pressure is 0.05～1MPa.
3. according to the method for described production ethene of claim 1 and propylene, it is characterized in that methyl alcohol and dme weight and ethanol weight ratio are 0.5～3: 1.
CN2006101178632A 2006-11-02 2006-11-02 Method for producing ethylene, propylene Active CN101172917B (en)

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DE102011013909A1 (en) 2011-03-15 2012-09-20 Süd-Chemie AG Process for the preparation of a zeolite based catalyst for the conversion of methanol to olefins

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1352627A (en) * 1999-09-23 2002-06-05 埃克森美孚石油公司 Process for converting methanol or dimethyl ether to olefins
CN1489563A (en) * 2001-02-16 2004-04-14 ����ɭ���ڻ�ѧר����˾ Method for converting oxygenate feed to olefin product

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1352627A (en) * 1999-09-23 2002-06-05 埃克森美孚石油公司 Process for converting methanol or dimethyl ether to olefins
CN1489563A (en) * 2001-02-16 2004-04-14 ����ɭ���ڻ�ѧר����˾ Method for converting oxygenate feed to olefin product

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