CN102875286A - Method for producing low-carbon olefins from methanol and naphtha - Google Patents
Method for producing low-carbon olefins from methanol and naphtha Download PDFInfo
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- CN102875286A CN102875286A CN201110195293XA CN201110195293A CN102875286A CN 102875286 A CN102875286 A CN 102875286A CN 201110195293X A CN201110195293X A CN 201110195293XA CN 201110195293 A CN201110195293 A CN 201110195293A CN 102875286 A CN102875286 A CN 102875286A
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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
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- Y02P20/50—Improvements relating to the production of bulk chemicals
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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
- Y02P20/584—Recycling of catalysts
Abstract
The invention relates to a method for producing low-carbon olefins from methanol and naphtha to mainly solve a low low-carbon olefin yield problem in previous technologies. The method mainly comprises the following steps: 1, allowing a naphtha-containing raw material to enter a first reaction zone and contact with a molecular sieve catalyst, allowing a generated gas phase material flow and a catalyst to contact with a raw material which mainly comprises methanol and enters from the distribution tube positioned at the outlet end of the first reaction zone, and then allowing the gas phase material flow to enter a second reaction zone to generate a product material flow comprising the low-carbon olefins and simultaneously form a catalyst to be regenerated; 2, dividing the catalyst to be regenerated into at least two parts, allowing one part of the catalyst to be regenerated to enter a regenerator for regeneration to form a regenerated catalyst, and allowing the other part of the catalyst to be regenerated to go through an outer circuiting incline tube and then return to the second reaction zone; and 3, returning the regenerated catalyst to the first reaction zone, wherein the methanol entering the from the distribution tube contacts with the gas phase material flow formed in the first reaction zone in a countercurrent manner, and the feed temperature of the raw material mainly comprising methanol is 40-200DEG C. The above technical scheme well solves the problem, and the method can be used for the industrial production of the low-carbon olefins.
Description
Technical field
The present invention relates to a kind of method of producing low-carbon alkene by methyl alcohol and petroleum naphtha.
Technical background
Low-carbon alkene, namely ethene and propylene are two kinds of important basic chemical industry raw materials, its demand is in continuous increase.Usually, ethene, propylene are to produce by petroleum path, but because limited supply and the higher price of petroleum resources, the cost of being produced ethene, propylene by petroleum resources constantly increases.In recent years, people begin to greatly develop the technology that alternative materials transforms ethene processed, propylene.Wherein, the important alternative materials that is used for light olefin production of one class is oxygenatedchemicals, such as alcohols (methyl alcohol, ethanol), ethers (dme, methyl ethyl ether), ester class (methylcarbonate, methyl-formiate) etc., these oxygenatedchemicalss can be transformed by coal, Sweet natural gas, biomass equal energy source.Some oxygenatedchemicals can reach fairly large production, such as methyl alcohol, can be made by coal or Sweet natural gas, and technique is very ripe, can realize up to a million tonnes industrial scale.Because the popularity in oxygenatedchemicals source, add and transform the economy that generates light olefin technique, so by the technique of oxygen-containing compound conversion to produce olefine (OTO), particularly the technique by preparing olefin by conversion of methanol (MTO) is subject to increasing attention.
Petroleum naphtha is a kind of light-end products, is cut corresponding cut and is got by crude distillation or oil secondary processing.Its boiling spread is decided according to need, is generally wider boiling range, such as 20-220 ℃.Petroleum naphtha is the pyrolysis in tubular furnace preparing ethylene, and propylene and catalytic reforming are produced the important source material of benzene,toluene,xylene.As cracking stock, require petroleum naphtha form in the content of alkane and naphthenic hydrocarbon be not less than 70% (volume).The naphtha catalytic pyrolysis preparing low-carbon alkene then is under the condition that catalyzer exists, and petroleum hydrocarbon is carried out the production process that cracking obtains low-carbon alkene.Compare with traditional tube furnace steam heat cracking, this process reaction temperature is than low 50～200 ℃ approximately of steam cracking reactions, and energy consumption significantly reduces; Cracking furnace pipe inwall coking rate also can reduce, thereby but prolong operation cycle increases the boiler tube life-span; Simultaneously Carbon emission also can reduce, and has alleviated pollution, and can adjust the product mix flexibly.
Technology and reactor that a kind of oxygenate conversion is low-carbon alkene have been announced among the US6166282, adopt fast fluidized bed reactor, gas phase is after the lower Mi Xiangfanyingqu reaction of gas speed is finished, after rising to the fast subregion that internal diameter diminishes rapidly, adopt special gas-solid separation equipment initial gross separation to go out most entrained catalyst.Because reaction after product gas and catalyzer sharp separation have effectively prevented the generation of secondary reaction.Through analog calculation, to compare with traditional bubbling fluidization bed bioreactor, this fast fluidized bed reactor internal diameter and the required reserve of catalyzer all greatly reduce.
The multiple riser reaction unit of having announced among the CN1723262 with central catalyst return is low-carbon alkene technique for oxygenate conversion, this covering device comprises a plurality of riser reactors, gas solid separation district, a plurality of offset components etc., each riser reactor has the port of injecting catalyst separately, be pooled to the disengaging zone of setting, catalyzer and gas product are separated.But there is the lower shortcoming of yield of light olefins in the method.
Announced a kind of method of methanol production propylene among EP0448000 and the EP0882692, methyl alcohol at first is converted into DME and water, then mixture is transported to the First reactor, and adds steam in this reactor.In the first reactor methyl alcohol with (or) dme or its mixture contact with catalyzer and react, catalyzer adopts the special-purpose ZSM-5 catalyzer that contains ZnO and CdO, 280～570 ℃ of temperature of reaction, pressure 0.01～0.1MPa prepares the product take propylene as main hydro carbons.Heavier product such as C
5 +The hydrocarbon continuation is reacted in second reactor and is converted into take propylene as main hydro carbons, sends separator back to after cooling.Product is compressed, can obtain purity after further refining is 97% chemical grade propylene.But adopt a plurality of fixed-bed reactor in this technique, because the restriction of the activity of catalyzer therefore need frequent blocked operation, and the heat-obtaining problem is also very complicated.
US 20070083071 has announced the processing method that a kind of hydrocarbon catalytic pyrolysis is produced ethene, propylene, hydrocarbon feed is converted into the product that comprises low-carbon alkene in catalytic cracker, then product stream is separated into C2～C3 alkane, C2～C3 alkene, three kinds of logistics of C4+ hydrocarbon by series of process, C2～C3 alkane is returned tube cracking furnace carry out thermo-cracking, the C4+ hydrocarbon returns catalytic cracker and carries out catalytic pyrolysis, finally obtains ethene, the propylene product of higher yields.The method adopts riser reactor, and reactant residence time is shorter, and low-carbon alkene product once through yield is lower.
Since the reaction of naphtha catalytic cracking and preparing olefin by conversion of methanol the purpose product---low-carbon alkene is identical, and the main ingredient kind in the product is roughly the same separately, the catalyst system that adopts is also roughly the same, and from the reaction mechanism angle, all have the process that is cracked into the small molecules hydro carbons by macromole hydrocarbon or intermediate, so these two kinds of Technologies are had ready conditions and are coupled.The present invention has solved this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the not high problem of yield of light olefins that exists in the prior art, and a kind of new method by methyl alcohol and petroleum naphtha production low-carbon alkene is provided.The method is used for the production of low-carbon alkene, has the higher advantage of yield of light olefins.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of method of producing low-carbon alkene by methyl alcohol and petroleum naphtha, mainly may further comprise the steps: (1) comprises that the raw material of petroleum naphtha enters the first reaction zone, contact with molecular sieve catalyst, the gaseous stream that generates and catalyzer with enter second reaction zone after the raw material that is mainly methyl alcohol that enters from the distribution pipe that is positioned at the first reaction zone exit end contacts, generation comprises the product stream of low-carbon alkene, forms simultaneously reclaimable catalyst; (2) described reclaimable catalyst is divided into two portions at least, and a part enters revivifier regeneration, forms regenerated catalyst, and a part is returned second reaction zone through the outer circulation inclined tube; (3) described regenerated catalyst returns the first reaction zone; Wherein, the gaseous stream that forms in methyl alcohol that described distribution pipe enters and the first reaction zone is counter current contact, and the described feeding temperature that is mainly the raw material of methyl alcohol is 40～200 ℃.
In the technique scheme, described catalyzer comprises ZSM-5 molecular sieve, SiO
2/ Al
2O
3Mol ratio is 10～100; Described regenerated catalyst coke content massfraction is 0.01～0.5%; Also comprise water vapour in described the first reaction zone feeds, the weight ratio of water vapour and petroleum naphtha is 0.05～1.5: 1; Described petroleum naphtha boiling range is between 20 ℃～220 ℃; Reaction conditions is in described the first reaction zone: temperature of reaction is 570～670 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 0.3～1.0 meter per second; Reaction conditions is in the second reaction zone: temperature of reaction is 500～600 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 1.0～4.0 meter per seconds; Described second reaction zone outlet arranges gas-solid sharp separation equipment; Described distribution pipe is dendriform; Described reclaimable catalyst is divided into two portions at least, and 40～80% weight enter revivifier regeneration, and 20～60% weight are returned second reaction zone through the outer circulation inclined tube.
Adopt method of the present invention, two reaction zones are set, it is low-carbon alkene that the first reaction zone is mainly used in naphtha catalytic cracking, the catalyzer of the first reaction zone is high temperature, the high activated catalyst from revivifier, second reaction zone is mainly used in catalyzed conversion methyl alcohol and the complete petroleum naphtha of unreacted, with production low-carbon alkene as much as possible.Methyl alcohol enters reaction zone and enters by distribution pipe, and distribution pipe material outlet opening direction deflection is lower, distribution pipe is arranged on the exit end of the first reaction zone, the gaseous stream of the methyl alcohol that enters and the first reaction zone presents counter current contact, effectively guaranteed the abundant good mixing of methyl alcohol and the first reaction zone gaseous stream, the methanol feeding temperature is lower simultaneously, and having reduced methanolysis is CO, H
2Probability.In addition, the first reaction zone plays the effect to the pre-carbon distribution of catalyzer in the second reaction zone simultaneously, has improved the selectivity of light olefin in the second reaction zone.Second reaction zone is owing to entering of cold methanol and entering of reclaimable catalyst simultaneously, and temperature of reaction reduces, and this has just reduced some by product (such as methane, CO, H
2Deng) generation.Therefore, adopt method of the present invention, can reach the purpose that improves yield of light olefins.
Adopt technical scheme of the present invention: described catalyzer comprises ZSM-5 molecular sieve, SiO
2/ Al
2O
3Mol ratio is 10～100; Described regenerated catalyst coke content massfraction is 0.01～0.5%; Also comprise water vapour in described the first reaction zone feeds, the weight ratio of water vapour and petroleum naphtha is 0.05～1.5: 1; Described petroleum naphtha boiling range is between 20 ℃～220 ℃; Reaction conditions is in described the first reaction zone: temperature of reaction is 570～670 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 0.3～1.0 meter per second; Reaction conditions is in the second reaction zone: temperature of reaction is 500～600 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 1.0～4.0 meter per seconds; Described second reaction zone outlet arranges gas-solid sharp separation equipment; Described distribution pipe is dendriform; Described reclaimable catalyst is divided into two portions at least, and 40～80% weight enter revivifier regeneration, and 20～60% weight are returned second reaction zone through the outer circulation inclined tube, and the low-carbon alkene carbon base absorption rate can reach 65.09% weight, has obtained preferably technique effect.
Description of drawings
Fig. 1 is the schematic flow sheet of device of the present invention;
Among Fig. 1,1 is the feed naphtha charging; 2 is feed distributing plate; 3 is distribution pipe; 4 is the first reaction zone; 5 is second reaction zone; 6 is catalyzer outer circulation inclined tube; 7 are gas-solid sharp separation equipment; 8 is gas-solid cyclone separator; 9 is the product stream outlet line; 10 is collection chamber; 11 is the methanol feedstock feeding line; 12 is regenerator sloped tube; 13 is settling vessel; 14 is inclined tube to be generated.
The raw material that comprises petroleum naphtha enters the first reaction zone 4, contact with molecular sieve catalyst, the gaseous stream that generates and catalyzer with enter second reaction zone 5 after the raw material that is mainly methyl alcohol that enters from the distribution pipe 3 that is positioned at the first reaction zone 4 exit end contacts, generation comprises the product stream of low-carbon alkene, through gas-solid sharp separation equipment 7, after separating, gas-solid cyclone separator 8 enters centrifugal station, isolated catalyzer is as reclaimable catalyst, reclaimable catalyst is divided into two portions at least, a part enters revivifier regeneration through inclined tube 14 to be generated, form regenerated catalyst, a part is returned second reaction zone 5 through outer circulation inclined tube 6, and the regenerated catalyst of formation returns the first reaction zone 4 through regenerator sloped tube 12.
The invention will be further elaborated below by embodiment, but be not limited only to present embodiment.
Embodiment
[embodiment 1]
In reaction unit as shown in Figure 1, catalyzer is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 10, petroleum naphtha and water vapour entered the first reaction zone take weight ratio as 1.5: 1, contact with catalyzer, the gaseous stream that generates and catalyzer with enter second reaction zone after the raw material that is mainly methyl alcohol that enters from the distribution pipe that is positioned at the first reaction zone exit end contacts, generation comprises the product stream of low-carbon alkene, form simultaneously reclaimable catalyst, reclaimable catalyst is divided into two portions, 40% weight enters revivifier regeneration, 60% weight is returned second reaction zone through the outer circulation inclined tube, and the regenerated catalyst that forms in the revivifier returns the first reaction zone.Wherein, the gaseous stream that forms in methyl alcohol that distribution pipe enters and the first reaction zone is counter current contact, and the feeding temperature of methanol feedstock is 200 ℃.Regenerated catalyst coke content massfraction is 0.01%, and described petroleum naphtha forms and sees Table that reaction conditions is in 1, the first reaction zone: temperature of reaction is 570 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and the gas phase linear speed is 0.3 meter per second; Reaction conditions is in the second reaction zone: temperature of reaction is 500 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and the gas phase linear speed is 1.0 meter per seconds, and the second reaction zone outlet arranges gas-solid sharp separation equipment, and distribution pipe is dendriform.Methyl alcohol is 1: 2 with the feed weight ratio of petroleum naphtha.Keep the stability of catalyst flow control, gas product adopts online gas chromatographic analysis, and the low-carbon alkene carbon base absorption rate is 54.79% weight.
Table 1 petroleum naphtha the typical case form
| Initial boiling point, ℃ | 40 |
| Final boiling point, ℃ | 162 |
| Positive structure and isoparaffin, % by weight | 65.18 |
| Alkene, % by weight | 0.17 |
| Naphthenic hydrocarbon, % by weight | 28.44 |
| Aromatic hydrocarbons, % by weight | 6.21 |
[embodiment 2]
According to embodiment 1 described condition and step, catalyzer is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 100, petroleum naphtha and water vapour entered the first reaction zone take weight ratio as 0.05: 1, contact with catalyzer, the gaseous stream that generates and catalyzer with enter second reaction zone after the raw material that is mainly methyl alcohol that enters from the distribution pipe that is positioned at the first reaction zone exit end contacts, generation comprises the product stream of low-carbon alkene, form simultaneously reclaimable catalyst, reclaimable catalyst is divided into two portions, 80% weight enters revivifier regeneration, 20% weight is returned second reaction zone through the outer circulation inclined tube, and the regenerated catalyst that forms in the revivifier returns the first reaction zone.Wherein, the gaseous stream that forms in methyl alcohol that distribution pipe enters and the first reaction zone is counter current contact, and the feeding temperature of methanol feedstock is 40 ℃.Regenerated catalyst coke content massfraction is that reaction conditions is in 0.5%, the first reaction zone: temperature of reaction is 670 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and the gas phase linear speed is 1.0 meter per seconds; Reaction conditions is in the second reaction zone: temperature of reaction is 600 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and the gas phase linear speed is 4.0 meter per seconds, and the second reaction zone outlet arranges gas-solid sharp separation equipment, and distribution pipe is dendriform.Methyl alcohol is 1: 1 with the feed weight ratio of petroleum naphtha.Keep the stability of catalyst flow control, gas product adopts online gas chromatographic analysis, and the low-carbon alkene carbon base absorption rate is 63.44% weight.
[embodiment 3]
According to embodiment 1 described condition and step, catalyzer is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 70, petroleum naphtha and water vapour entered the first reaction zone take weight ratio as 0.5: 1, reclaimable catalyst is divided into two portions, and 50% weight enters revivifier regeneration, 50% weight is returned second reaction zone through the outer circulation inclined tube, and the feeding temperature of methanol feedstock is 100 ℃.Regenerated catalyst coke content massfraction is that reaction conditions is in 0.1%, the first reaction zone: temperature of reaction is 650 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and the gas phase linear speed is 0.6 meter per second; Reaction conditions is in the second reaction zone: temperature of reaction is 617 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and the gas phase linear speed is 1.5 meter per seconds, and methyl alcohol is 1: 1 with the feed weight ratio of petroleum naphtha.Keep the stability of catalyst flow control, gas product adopts online gas chromatographic analysis, and the low-carbon alkene carbon base absorption rate is 65.09% weight.
[embodiment 4]
According to embodiment 1 described condition and step, catalyzer is ZSM-5, SiO
2/ Al
2O
3Mol ratio is 70, petroleum naphtha and water vapour entered the first reaction zone take weight ratio as 0.5: 1, reclaimable catalyst is divided into two portions, and 60% weight enters revivifier regeneration, 40% weight is returned second reaction zone through the outer circulation inclined tube, and the feeding temperature of methanol feedstock is 80 ℃.Regenerated catalyst coke content massfraction is that reaction conditions is in 0.1%, the first reaction zone: temperature of reaction is 657 ℃, and reaction pressure is counted 0.3MPa with gauge pressure, and the gas phase linear speed is 0.51 meter per second; Reaction conditions is in the second reaction zone: temperature of reaction is 626 ℃, and reaction pressure is counted 0.3MPa with gauge pressure, and the gas phase linear speed is 1.25 meter per seconds, and methyl alcohol is 1: 1 with the feed weight ratio of petroleum naphtha.Keep the stability of catalyst flow control, gas product adopts online gas chromatographic analysis, and the low-carbon alkene carbon base absorption rate is 62.03% weight.
[comparative example 1]
According to embodiment 1 described condition and step, just do not distinguish first, second reaction zone, after mixing, methyl alcohol and feed naphtha enter reaction zone from the reaction zone bottom, the reclaimable catalyst that comes from the catalyzer outer circulating tube returns the reaction zone bottom, regenerated catalyst returns the reaction zone bottom, and the low-carbon alkene carbon base absorption rate is 50.43% weight.
Obviously, adopt method of the present invention, can reach the purpose that improves yield of light olefins, have larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (9)
1. method of producing low-carbon alkene by methyl alcohol and petroleum naphtha mainly may further comprise the steps:
(1) raw material that comprises petroleum naphtha enters the first reaction zone, contact with molecular sieve catalyst, the gaseous stream that generates and catalyzer with enter second reaction zone after the raw material that is mainly methyl alcohol that enters from the distribution pipe that is positioned at the first reaction zone exit end contacts, generation comprises the product stream of low-carbon alkene, forms simultaneously reclaimable catalyst;
(2) described reclaimable catalyst is divided into two portions at least, and a part enters revivifier regeneration, forms regenerated catalyst, and a part is returned second reaction zone through the outer circulation inclined tube;
(3) described regenerated catalyst returns the first reaction zone;
Wherein, the gaseous stream that forms in methyl alcohol that described distribution pipe enters and the first reaction zone is counter current contact, and the described feeding temperature that is mainly the raw material of methyl alcohol is 40～200 ℃.
2. described method of producing low-carbon alkene by methyl alcohol and petroleum naphtha according to claim 1 is characterized in that described catalyzer comprises ZSM-5 molecular sieve, SiO
2/ Al
2O
3Mol ratio is 10～100.
3. described method of producing low-carbon alkene by methyl alcohol and petroleum naphtha according to claim 1 is characterized in that described regenerated catalyst coke content massfraction is 0.01～0.5%.
4. described method of producing low-carbon alkene by methyl alcohol and petroleum naphtha according to claim 1 is characterized in that also comprising water vapour in described the first reaction zone feeds that the weight ratio of water vapour and petroleum naphtha is 0.05～1.5: 1.
5. described method of producing low-carbon alkene by methyl alcohol and petroleum naphtha according to claim 1 is characterized in that described petroleum naphtha boiling range is between 20 ℃～220 ℃.
6. described method of being produced low-carbon alkene by methyl alcohol and petroleum naphtha according to claim 1, it is characterized in that reaction conditions is in described the first reaction zone: temperature of reaction is 570～670 ℃, reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 0.3～1.0 meter per second; Reaction conditions is in the second reaction zone: temperature of reaction is 500～600 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 1.0～4.0 meter per seconds.
7. described method of producing low-carbon alkene by methyl alcohol and petroleum naphtha according to claim 1 is characterized in that described second reaction zone outlet arranges gas-solid sharp separation equipment.
8. described method of producing low-carbon alkene by methyl alcohol and petroleum naphtha according to claim 1 is characterized in that described distribution pipe is dendriform.
9. described method of producing low-carbon alkene by methyl alcohol and petroleum naphtha according to claim 1 is characterized in that reclaimable catalyst is divided into two portions at least, and 40～80% weight enter revivifier regeneration, and 20～60% weight are returned second reaction zone through the outer circulation inclined tube.
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| CN111233608A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Naphtha-containing raw material conversion method |
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