CN102875286B - 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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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 being produced low-carbon alkene by methyl alcohol and petroleum naphtha.
Technical background
Low-carbon alkene, i.e. ethene and propylene, be two kinds of important basic chemical industry raw materials, its demand is in continuous increase.Usually, ethene, propylene are produced by petroleum path, but due to the limited supply of petroleum resources and higher price, produce ethene by petroleum resources, the cost of propylene constantly increases.In recent years, people start to greatly develop the technology that alternative materials transforms ethene processed, propylene.Wherein, the important alternative materials 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, and as methyl alcohol, can be obtained by coal or Sweet natural gas, technique is very ripe, can realize the industrial scale of up to a million tonnes.Due to the popularity in oxygenatedchemicals source, add the economy transforming and generate light olefin technique, so by the technique of oxygen-containing compound conversion to produce olefine (OTO), be particularly subject to increasing attention by the technique of preparing olefin by conversion of methanol (MTO).
Petroleum naphtha is a kind of light-end products, is cut corresponding cut by crude distillation or oil secondary processing and is obtained.Its boiling spread is determined according to need, is generally wider boiling range, as 20-220 DEG C.Petroleum naphtha is pyrolysis in tubular furnace preparing ethylene, and propylene and catalytic reforming produce the important source material of benzene,toluene,xylene.As cracking stock, in requiring petroleum naphtha to form, the content of alkane and naphthenic hydrocarbon is not less than 70% (volume).Naphtha catalytic pyrolysis preparing low-carbon alkene is then under catalyzer existent condition, carries out cracking to obtain the production process of low-carbon alkene to petroleum hydrocarbon.Compare with traditional tube furnace steam heat cracking, this process reaction temperature is about lower than steam cracking reaction 50 ~ 200 DEG C, and energy consumption significantly reduces; Cracking furnace pipe inwall coking rate also can reduce, thus can prolong operation cycle, increases the boiler tube life-span; Carbon emission simultaneously also can reduce, and alleviates pollution, and can adjust the product mix flexibly.
Technology and reactor that a kind of oxygenate conversion is low-carbon alkene is disclosed in US6166282, adopt fast fluidized bed reactor, gas phase is after the lower Mi Xiangfanyingqu of gas speed has reacted, after rising to the fast subregion that internal diameter diminishes rapidly, special gas-solid separation equipment initial gross separation is adopted to go out most entrained catalyst.Due to reaction after product gas and catalyzer sharp separation, effectively prevent the generation of secondary reaction.Through analog calculation, compared with traditional bubbling fluidization bed bioreactor, needed for this fast fluidized bed reactor internal diameter and catalyzer, reserve all greatly reduces.
The multiple riser reaction unit disclosed in CN1723262 with central catalyst return is low-carbon alkene technique for oxygenate conversion, this covering device comprises multiple riser reactor, gas solid separation district, multiple 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.
Disclose a kind of method of methanol production propylene in EP0448000 and EP0882692, first methyl alcohol be converted into DME and water, then mixture is transported to First reactor, and add steam in this reactor.In the first reactor, methyl alcohol and (or) dme or its mixture and catalyst exposure react, catalyzer adopts the special ZSM-5 catalyzer containing ZnO and CdO, temperature of reaction 280 ~ 570 DEG C, pressure 0.01 ~ 0.1MPa, preparing with propylene is the product of main hydro carbons.Heavier product is as C
5 +hydrocarbon continues to carry out reacting the hydro carbons be converted into based on propylene in second reactor, after cooling, send separator back to.Product is compressed, refining further after can obtain the chemical grade propylene that purity is 97%.But adopt multiple fixed-bed reactor in this technique, because the activity of catalyzer limits, therefore need frequent blocked operation, and heat-obtaining problem is also very complicated.
US 20070083071 discloses the processing method that a kind of hydrocarbon catalytic pyrolysis produces ethene, propylene, hydrocarbon feed is converted into the product comprising low-carbon alkene in catalytic cracker, then product stream is separated into C2 ~ C3 alkane, C2 ~ C3 alkene, the three kinds of logistics of C4+ hydrocarbon by series of process, C2 ~ C3 alkane is returned tube cracking furnace and carries out thermo-cracking, C4+ hydrocarbon returns catalytic cracker and carries out catalytic pyrolysis, finally obtains the ethene of higher yields, propylene product.The method adopts riser reactor, and reactant residence time is shorter, and low-carbon alkene product once through yield is lower.
Due to naphtha catalytic cracking and preparing olefin by conversion of methanol react object product---low-carbon alkene is identical, and main ingredient kind separately in product is roughly the same, the catalyst system adopted is also roughly the same, and from reaction mechanism angle, all there is the process being cracked into small molecules hydro carbons by macromole hydrocarbon or intermediate, therefore these two kinds of Technologies are had ready conditions and are coupled.The present invention solves this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the problem that the yield of light olefins that exists in prior art is not high, provides a kind of method of being produced low-carbon alkene by methyl alcohol and petroleum naphtha newly.The method is used for, in the production of low-carbon alkene, having the advantage that yield of light olefins is higher.
For solving the problem, the technical solution used in the present invention is as follows: a kind of method of being produced low-carbon alkene by methyl alcohol and petroleum naphtha, mainly comprise the following steps: the raw material that (1) comprises petroleum naphtha enters the first reaction zone, contact with molecular sieve catalyst, generate gaseous stream and catalyzer and from the distribution pipe being positioned at the first reaction zone exit end enter be mainly the contact raw of methyl alcohol after enter second reaction zone, generate the product stream comprising low-carbon alkene, form reclaimable catalyst simultaneously; (2) described reclaimable catalyst is at least divided into two portions, and a part enters revivifier regeneration, forms regenerated catalyst, and a part returns to second reaction zone through outer circulation inclined tube; (3) described regenerated catalyst returns to the first reaction zone; Wherein, the gaseous stream formed in the methyl alcohol entered through described distribution pipe and the first reaction zone is counter current contact, described in be mainly the raw material of methyl alcohol feeding temperature be 40 ~ 200 DEG C.
In 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 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 DEG C ~ 220 DEG C; In described first reaction zone, reaction conditions is: temperature of reaction is 570 ~ 670 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 0.3 ~ 1.0 meter per second; In second reaction zone, reaction conditions is: temperature of reaction is 500 ~ 600 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 1.0 ~ 4.0 meter per seconds; The outlet of described second reaction zone arranges gas-solid sharp separation equipment; Described distribution pipe is dendriform; Described reclaimable catalyst is at least divided into two portions, and 40 ~ 80% weight enter revivifier regeneration, and 20 ~ 60% weight return to second reaction zone through outer circulation inclined tube.
Adopt method of the present invention, two reaction zones is set, it is low-carbon alkene that first reaction zone is mainly used in naphtha catalytic cracking, the catalyzer of the first reaction zone is high temperature, high activated catalyst from revivifier, second reaction zone is mainly used in catalyzed conversion methyl alcohol and the complete petroleum naphtha of unreacted, with as far as possible many production low-carbon alkenes.Methyl alcohol is entered reaction zone and is entered by distribution pipe, and under distribution pipe material outlet opening direction deflection, distribution pipe is arranged on the exit end of the first reaction zone, the gaseous stream of the methyl alcohol entered and the first reaction zone presents counter current contact, effectively ensure that the abundant good mixing of methyl alcohol and the first reaction zone gaseous stream, methanol feeding temperature is lower simultaneously, and decreasing methanolysis is CO, H
2probability.In addition, the first reaction zone is played to the effect of the pre-carbon distribution of the catalyzer in second reaction zone simultaneously, improves the selectivity of light olefin in second reaction zone.Second reaction zone is due to entering of cold methanol and entering of reclaimable catalyst simultaneously, and temperature of reaction reduces, and this reduces some by product (as methane, CO, H
2deng) generation.Therefore, adopt method of the present invention, the object improving yield of light olefins can be reached.
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 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 DEG C ~ 220 DEG C; In described first reaction zone, reaction conditions is: temperature of reaction is 570 ~ 670 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 0.3 ~ 1.0 meter per second; In second reaction zone, reaction conditions is: temperature of reaction is 500 ~ 600 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 1.0 ~ 4.0 meter per seconds; The outlet of described second reaction zone arranges gas-solid sharp separation equipment; Described distribution pipe is dendriform; Described reclaimable catalyst is at least divided into two portions, and 40 ~ 80% weight enter revivifier regeneration, and 20 ~ 60% weight return to second reaction zone through outer circulation inclined tube, and low-carbon alkene carbon base absorption rate can reach 65.09% weight, achieve good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of device of the present invention;
In Fig. 1,1 is 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 external catalyst circulation inclined tube; 7 is gas-solid sharp separation equipment; 8 is gas-solid cyclone separator; 9 is product stream outlet line; 10 is collection chamber; 11 is methanol feedstock feeding line; 12 is regenerator sloped tube; 13 is settling vessel; 14 is inclined tube to be generated.
The raw material comprising petroleum naphtha enters the first reaction zone 4, contact with molecular sieve catalyst, generate gaseous stream and catalyzer and from the distribution pipe 3 being positioned at the first reaction zone 4 exit end enter be mainly the contact raw of methyl alcohol after enter second reaction zone 5, generate the product stream comprising low-carbon alkene, through gas-solid sharp separation equipment 7, gas-solid cyclone separator 8 enters centrifugal station after being separated, isolated catalyzer is as reclaimable catalyst, reclaimable catalyst is at least divided into two portions, a part enters revivifier regeneration through inclined tube 14 to be generated, form regenerated catalyst, a part returns to second reaction zone 5 through outer circulation inclined tube 6, the regenerated catalyst formed returns to the first reaction zone 4 through regenerator sloped tube 12.
Below by embodiment, the invention will be further elaborated, but be not limited only to the 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 are enter first reaction zone at 1.5: 1 with weight ratio, with catalyst exposure, generate gaseous stream and catalyzer and from the distribution pipe being positioned at the first reaction zone exit end enter be mainly the contact raw of methyl alcohol after enter second reaction zone, generate the product stream comprising low-carbon alkene, form reclaimable catalyst simultaneously, reclaimable catalyst is divided into two portions, 40% weight enters revivifier regeneration, 60% weight returns to second reaction zone through outer circulation inclined tube, and the regenerated catalyst formed in revivifier returns to the first reaction zone.Wherein, the gaseous stream formed in the methyl alcohol entered through distribution pipe and the first reaction zone is counter current contact, and the feeding temperature of methanol feedstock is 200 DEG C.Regenerated catalyst coke content massfraction is 0.01%, and described petroleum naphtha composition is in table 1, and in the first reaction zone, reaction conditions is: temperature of reaction is 570 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 0.3 meter per second; In second reaction zone, reaction conditions is: temperature of reaction is 500 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 1.0 meter per seconds, and 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 low-carbon alkene carbon base absorption rate is 54.79% weight.
Table 1 petroleum naphtha typical case composition
| Initial boiling point, DEG C | 40 |
| Final boiling point, DEG C | 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 the condition described in embodiment 1 and step, catalyzer is ZSM-5, SiO
2/ Al
2o
3mol ratio is 100, petroleum naphtha and water vapour are enter first reaction zone at 0.05: 1 with weight ratio, with catalyst exposure, generate gaseous stream and catalyzer and from the distribution pipe being positioned at the first reaction zone exit end enter be mainly the contact raw of methyl alcohol after enter second reaction zone, generate the product stream comprising low-carbon alkene, form reclaimable catalyst simultaneously, reclaimable catalyst is divided into two portions, 80% weight enters revivifier regeneration, 20% weight returns to second reaction zone through outer circulation inclined tube, and the regenerated catalyst formed in revivifier returns to the first reaction zone.Wherein, the gaseous stream formed in the methyl alcohol entered through distribution pipe and the first reaction zone is counter current contact, and the feeding temperature of methanol feedstock is 40 DEG C.Regenerated catalyst coke content massfraction is that in the 0.5%, first reaction zone, reaction conditions is: temperature of reaction is 670 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 1.0 meter per seconds; In second reaction zone, reaction conditions is: temperature of reaction is 600 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 4.0 meter per seconds, and 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 low-carbon alkene carbon base absorption rate is 63.44% weight.
[embodiment 3]
According to the condition described in embodiment 1 and step, catalyzer is ZSM-5, SiO
2/ Al
2o
3mol ratio is 70, petroleum naphtha and water vapour are enter first reaction zone at 0.5: 1 with weight ratio, and reclaimable catalyst is divided into two portions, and 50% weight enters revivifier regeneration, 50% weight returns to second reaction zone through outer circulation inclined tube, and the feeding temperature of methanol feedstock is 100 DEG C.Regenerated catalyst coke content massfraction is that in the 0.1%, first reaction zone, reaction conditions is: temperature of reaction is 650 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 0.6 meter per second; In second reaction zone, reaction conditions is: temperature of reaction is 617 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and 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 low-carbon alkene carbon base absorption rate is 65.09% weight.
[embodiment 4]
According to the condition described in embodiment 1 and step, catalyzer is ZSM-5, SiO
2/ Al
2o
3mol ratio is 70, petroleum naphtha and water vapour are enter first reaction zone at 0.5: 1 with weight ratio, and reclaimable catalyst is divided into two portions, and 60% weight enters revivifier regeneration, 40% weight returns to second reaction zone through outer circulation inclined tube, and the feeding temperature of methanol feedstock is 80 DEG C.Regenerated catalyst coke content massfraction is that in the 0.1%, first reaction zone, reaction conditions is: temperature of reaction is 657 DEG C, and reaction pressure counts 0.3MPa with gauge pressure, and gas phase linear speed is 0.51 meter per second; In second reaction zone, reaction conditions is: temperature of reaction is 626 DEG C, and reaction pressure counts 0.3MPa with gauge pressure, and 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 low-carbon alkene carbon base absorption rate is 62.03% weight.
[comparative example 1]
According to the condition described in embodiment 1 and step, just do not distinguish first, second reaction zone, bottom reaction zone, reaction zone is entered after methyl alcohol and feed naphtha mixing, the reclaimable catalyst come from external catalyst circulation pipe returns bottom reaction zone, regenerated catalyst returns bottom reaction zone, and low-carbon alkene carbon base absorption rate is 50.43% weight.
Obviously, adopt method of the present invention, the object improving yield of light olefins can be reached, there is larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (7)
1. produced a method for low-carbon alkene by methyl alcohol and petroleum naphtha, mainly comprise the following steps:
(1) raw material comprising petroleum naphtha enters the first reaction zone, contact with molecular sieve catalyst, generate gaseous stream and catalyzer and from the distribution pipe being positioned at the first reaction zone exit end enter be mainly the contact raw of methyl alcohol after enter second reaction zone, generate the product stream comprising low-carbon alkene, form reclaimable catalyst simultaneously;
(2) described reclaimable catalyst is at least divided into two portions, and a part enters revivifier regeneration, forms regenerated catalyst, and a part returns to second reaction zone through outer circulation inclined tube;
(3) described regenerated catalyst returns to the first reaction zone;
Wherein, the gaseous stream formed in the methyl alcohol entered through described distribution pipe and the first reaction zone is counter current contact, described in be mainly the raw material of methyl alcohol feeding temperature be 40 ~ 200 DEG C; Described catalyzer comprises ZSM-5 molecular sieve, SiO
2/ Al
2o
3mol ratio is 10 ~ 100; Also comprise water vapour in described first reaction zone feeds, the weight ratio of water vapour and petroleum naphtha is 0.05 ~ 1.5: 1.
2. produced the method for low-carbon alkene according to claim 1 by methyl alcohol and petroleum naphtha, it is characterized in that described regenerated catalyst coke content massfraction is 0.01 ~ 0.5%.
3. produced the method for low-carbon alkene according to claim 1 by methyl alcohol and petroleum naphtha, it is characterized in that described petroleum naphtha boiling range is between 20 DEG C ~ 220 DEG C.
4. the method for low-carbon alkene is produced according to claim 1 by methyl alcohol and petroleum naphtha, it is characterized in that in described first reaction zone, reaction conditions is: temperature of reaction is 570 ~ 670 DEG C, reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 0.3 ~ 1.0 meter per second; In second reaction zone, reaction conditions is: temperature of reaction is 500 ~ 600 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 1.0 ~ 4.0 meter per seconds.
5. produced the method for low-carbon alkene according to claim 1 by methyl alcohol and petroleum naphtha, it is characterized in that the outlet of described second reaction zone arranges gas-solid sharp separation equipment.
6. produced the method for low-carbon alkene according to claim 1 by methyl alcohol and petroleum naphtha, it is characterized in that described distribution pipe is dendriform.
7. produced the method for low-carbon alkene according to claim 1 by methyl alcohol and petroleum naphtha, it is characterized in that reclaimable catalyst is at least divided into two portions, 40 ~ 80% weight enter revivifier regeneration, and 20 ~ 60% weight return to second reaction zone through outer circulation inclined tube.
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