CN103739419A - Method of preparing low-carbon olefins from methanol - Google Patents
Method of preparing low-carbon olefins from methanol Download PDFInfo
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- CN103739419A CN103739419A CN201210392999.XA CN201210392999A CN103739419A CN 103739419 A CN103739419 A CN 103739419A CN 201210392999 A CN201210392999 A CN 201210392999A CN 103739419 A CN103739419 A CN 103739419A
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Abstract
The invention relates to a method of preparing low-carbon olefins from methanol, mainly solving a problem that the yield of low-carbon olefins is low in the prior art. According to the technical scheme adopted by the method, the method comprises steps of: (a) feeding raw materials which are mainly methanol into a reaction zone, contacting the raw materials with a catalyst containing silicon-aluminum-phosphorus molecular sieve, subjecting a produced gas-phase stream and the catalyst to gas solid separation, allowing the separated gas-phase stream to enter into a separation process, and dividing the separated catalyst into at least two steams, wherein the first steam of the catalyst is returned to the reaction zone after heat exchange with an external cooler and the second steam of the catalyst is fed into a regenerator to be regenerated to form a regenerated catalyst; and (b) feeding the regenerated catalyst, after being degassed in a degassing section, into the external cooler to be mixed with the first steam of the catalyst and allowing the mixture to enter into the reaction zone, wherein the degassing zone is disposed below the regenerator, and the regenerated catalyst enters into a conveying pipe through a regeneration standpipe and enters into the external cooler under conveyance by a conveying medium. By the technical scheme, the problem is solved well and the method can be used in industrial production of the low-carbon olefins.
Description
Technical field
The present invention relates to a kind of method of preparing light olefins from methanol.
Background technology
Low-carbon alkene, i.e. ethene and propylene, is 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 due to the limited supply of petroleum resources and higher price, the cost of being produced ethene, propylene by petroleum resources constantly increases.In recent years, people start to greatly develop the technology of alternative materials conversion ethene processed, propylene.Wherein, the important alternative materials of producing for low-carbon alkene 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, as methyl alcohol, can be made by coal or Sweet natural gas, and technique is very ripe, can realize the industrial scale of up to a million tonnes.Due to the popularity in oxygenatedchemicals source, add and transform the economy that generates low-carbon alkene 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).
In US4499327 patent, silicoaluminophosphamolecular molecular sieve catalyst is applied to preparing olefin by conversion of methanol technique and studies in detail, think that SAPO-34 is the first-selected catalyzer of MTO technique.SAPO-34 catalyzer has very high selectivity of light olefin, and activity is also higher, and can make methanol conversion is reaction times of low-carbon alkene to be less than the degree of 10 seconds, more even reaches in the reaction time range of riser tube.
Technology and reactor that a kind of methanol conversion is low-carbon alkene in US 6166282, have been announced, adopt fast fluidized bed reactor, gas phase is after the lower Mi Xiangfanyingqu of gas speed has reacted, rise to after the fast subregion that internal diameter diminishes rapidly, adopt special gas-solid separation equipment initial gross separation to go out most entrained catalyst.Due to reaction after product gas and catalyzer sharp separation, effectively prevented the generation of secondary reaction.Through analog calculation, compared with traditional bubbling fluidization bed bioreactor, this fast fluidized bed reactor internal diameter and the required reserve of catalyzer all greatly reduce.But in the method, low-carbon alkene carbon base absorption rate is general all in 77% left and right, has the problem that yield of light olefins is lower.
In CN 1723262, having announced with the multiple riser reaction unit of central catalyst return is low-carbon alkene technique for oxygenate conversion, this covering device comprises multiple riser reactors, 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.In the method, low-carbon alkene carbon base absorption rate is general all between 75~80%, has equally the problem that yield of light olefins is lower.
All there is the problem that yield of light olefins is lower in prior art, the present invention has solved this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the lower problem of yield of light olefins existing in prior art, and a kind of method of new preparing light olefins from methanol is provided.The method, for the production of low-carbon alkene, has advantages of that yield of light olefins is higher.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of method of preparing light olefins from methanol, comprise the following steps: the raw material that (a) is mainly methyl alcohol enters reaction zone, contact with the catalyzer that comprises sial phosphorus molecular sieve, the gaseous stream generating and catalyzer are after gas solid separation, gaseous stream enters centrifugal station, isolated catalyzer is at least divided into two strands, first strand of catalyzer returns to reaction zone after external warmer heat exchange, second strand enters revivifier regeneration, forms regenerated catalyst; (b) described regenerated catalyst enters described external warmer after degas zone is degassed, and enters reaction zone after described first burst of catalyst mix; Wherein, described degas zone is positioned at revivifier below, and regenerated catalyst enters transfer lime through standpipe, enters described external warmer under the conveying of delivery medium.
In technique scheme, described sial phosphorus molecular sieve comprises SAPO-34; Described delivery medium is water vapour, comprise at least one in the hydrocarbon mixture of C4 alkene, and in described hydrocarbon mixture, C4 alkene mass content is greater than 60%; Described reaction zone reaction conditions is: temperature of reaction is 400~550 ℃, and reaction pressure is counted 0.01~0.3MPa with gauge pressure, and gas phase linear speed is 0.4~3 meter per second; The average carbon deposition quantity massfraction of described regenerated catalyst is 0.01~0.5%; Described isolated catalyzer is at least divided into two strands, and first strand of catalyzer accounts for 40~80% in massfraction, and second strand accounts for 20-60% in massfraction.
The method of calculation of average coke content of the present invention are that carbon deposit quality on catalyzer is divided by described catalyst quality.Carbon deposit measuring method on catalyzer is as follows: will mix the catalyst mix with carbon deposit comparatively uniformly, then weigh the band C catalyst of 0.1~1 gram, be put in pyrocarbon analyser and burn, by infrared analysis burn generate carbonic acid gas quality, thereby obtain the carbonaceous amount on catalyzer.
The preparation method of sial phosphorus molecular sieve of the present invention is: first preparing molecular sieve presoma, is 0.03~0.6R by mole proportioning: (Si 0.01~0.98: Al 0.01~0.6: P 0.01~0.6): 2~500 H
2o, wherein R represents template, and template is triethylamine, and constitutive material mixed solution obtains at the temperature of 100-250 ℃ after the crystallization of 1~10 hour; Again, molecular sieve presoma, phosphorus source, silicon source, aluminium source, template, water etc. are mixed according to certain ratio after at 110~260 ℃ hydrothermal crystallizing after at least 0.1 hour, finally obtain SAPO molecular sieve.The molecular sieve of preparation is mixed with the binding agent of required ratio, after the operation stepss such as, roasting dry through spraying, obtain final SAPO catalyzer, the weight percentage of binding agent in molecular sieve is between 10~90%.
Adopt method of the present invention, regenerated catalyst is entered to external warmer under the conveying of delivery medium, delivery medium preferably includes the hydrocarbon mixture of C4 alkene, and hydrocarbon mixture contact high temperature, highly active regenerated catalyst, can be cracked into low-carbon alkene.Meanwhile, external warmer, except playing the effect of heat exchange, also plays the effect of regenerated catalyst and reclaimable catalyst mixing tank, the catalyzer mixing returns to reaction zone, can make bottom, reaction zone catalyst mix even, reduce methanolysis probability, reach the object that improves yield of light olefins.In addition, the degas zone of revivifier is positioned at revivifier below, and then regenerated catalyst enters transfer lime through standpipe, and regenerated catalyst enters external warmer under the conveying of carrying strength, the layout of obvious this revivifier can reduce the layout height of revivifier, improves inclined tube impellent to be generated.
Adopt technical scheme of the present invention: described sial phosphorus molecular sieve comprises SAPO-34; Described delivery medium is water vapour, comprise at least one in the hydrocarbon mixture of C4 alkene, and in described hydrocarbon mixture, C4 alkene mass content is greater than 60%; Described reaction zone reaction conditions is: temperature of reaction is 400~550 ℃, and reaction pressure is counted 0.01~0.3MPa with gauge pressure, and gas phase linear speed is 0.4~3 meter per second; The average carbon deposition quantity massfraction of described regenerated catalyst is 0.01~0.5%; Described isolated catalyzer is at least divided into two strands, first strand of catalyzer accounts for 40~80% in massfraction, second strand accounts for 20-60% in massfraction, low-carbon alkene carbon base absorption rate reaches 84.78% (weight), than the low-carbon alkene carbon base absorption rate of prior art, exceed and can reach more than 3 percentage points, obtained good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for the invention;
In Fig. 1,1 is methanol feed line; 2 is reaction zone; 3 is gas-solid sharp separation equipment; 4 is stripping zone; 5 is inclined tube to be generated; 6 for entering external warmer inclined tube; 7 is external warmer lower oblique tube; 8 is cyclonic separator; 9 is negative area; 10 is the gaseous phase outlet of cyclonic separator 11; 11 is cyclonic separator; 12 is external warmer gaseous phase outlet; 13 is external warmer; 14 is external warmer fluidizing medium entrance; 15 is heat production coil pipe; 16 is transfer lime; 17 is delivery medium; 18 is standpipe; 19 is degassed medium; 20 is degas zone; 21 is grid distributor; 22 is regenerating medium; 23 is breeding blanket; 24 is revivifier negative area; 25 is cyclonic separator; 26 is exhanst gas outlet; 27 is product gas outlet pipeline.
The first strand of raw material that is mainly methyl alcohol enters reaction zone 2, contact with the catalyzer that comprises sial phosphorus molecular sieve, after the gaseous stream generating and catalyzer enter gas-solid sharp separation equipment 3, cyclonic separator 8, enter centrifugal station, catalyzer enters stripping zone 4, forms reclaimable catalyst; The reclaimable catalyst of stripping zone 4 is at least divided into two portions, a part enters external warmer 13, a part enters revivifier breeding blanket 23 through inclined tube 5 to be generated and regenerates, form regenerated catalyst, regenerated catalyst enters transfer lime 16 through standpipe 18 after degas zone 20 is degassed, then enters external warmer 13.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
On reaction unit as shown in Figure 1, purity is that the methyl alcohol of 99.5% (weight) enters reaction zone, contact with the catalyzer that comprises SAPO-34 molecular sieve, the gaseous stream generating enters centrifugal station after gas solid separation, catalyzer is divided into two portions after stripping, in massfraction, 80% enters external warmer, 20% enters revivifier regeneration, form regenerated catalyst, regenerated catalyst enters transfer lime through standpipe after degassed, contacts with delivery medium, and regenerated catalyst is delivered into external warmer.Delivery medium is water vapour, and reaction zone reaction conditions is: temperature of reaction is 550 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and gas phase linear speed is 3 meter per seconds, and the average carbon deposition quantity massfraction of regenerated catalyst is 0.5%.Reactor product adopts online gas chromatographic analysis, and low-carbon alkene carbon base absorption rate is 81.95% (weight).
[embodiment 2]
According to condition and step described in embodiment 1, catalyzer is divided into two portions after stripping, in massfraction, 40% enters external warmer, and 60% enters revivifier regeneration, forms regenerated catalyst, delivery medium is the hydrocarbon mixture that comprises C4 alkene, and in described hydrocarbon mixture, C4 alkene mass content is 61%.Reaction zone reaction conditions is: temperature of reaction is 400 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and gas phase linear speed is 0.4 meter per second, and the average carbon deposition quantity massfraction of regenerated catalyst is 0.015%.Reactor product adopts online gas chromatographic analysis, and low-carbon alkene carbon base absorption rate is 81.35% (weight).
[embodiment 3]
According to condition and step described in embodiment 2, catalyzer is divided into two portions after stripping, in massfraction, 60% enters external warmer, and 40% enters revivifier regeneration, forms regenerated catalyst, delivery medium is the hydrocarbon mixture that comprises C4 alkene, and in described hydrocarbon mixture, C4 alkene mass content is 92%.Reaction zone reaction conditions is: temperature of reaction is 480 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and gas phase linear speed is 1.3 meter per seconds, and the average carbon deposition quantity massfraction of regenerated catalyst is 0.1%.Reactor product adopts online gas chromatographic analysis, and low-carbon alkene carbon base absorption rate is 84.78% (weight).
[embodiment 4]
According to condition and step described in embodiment 3, catalyzer is divided into two portions after stripping, in massfraction, 50% enters external warmer, and 50% enters revivifier regeneration, forms regenerated catalyst, delivery medium is the hydrocarbon mixture that comprises C4 alkene, and in described hydrocarbon mixture, C4 alkene mass content is 76%.Reaction zone reaction conditions is: temperature of reaction is 500 ℃, and reaction pressure is counted 0.3MPa with gauge pressure, and gas phase linear speed is 0.8 meter per second, and the average carbon deposition quantity massfraction of regenerated catalyst is 0.05%.Reactor product adopts online gas chromatographic analysis, and low-carbon alkene carbon base absorption rate is 82.87% (weight).
[comparative example 1]
According to condition and step described in embodiment 3, regenerated catalyst directly returns to reaction zone, and yield of light olefins is 81.53% (weight).
Obviously, adopt method of the present invention, can reach the object that improves yield of light olefins, there is larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (9)
1. a method for preparing light olefins from methanol, comprises the following steps:
(a) raw material that is mainly methyl alcohol enters reaction zone, contact with the catalyzer that comprises sial phosphorus molecular sieve, the gaseous stream generating and catalyzer are after gas solid separation, gaseous stream enters centrifugal station, isolated catalyzer is at least divided into two strands, first strand of catalyzer returns to reaction zone after external warmer heat exchange, and second strand enters revivifier regeneration, form regenerated catalyst;
(b) described regenerated catalyst enters described external warmer after degas zone is degassed, and enters reaction zone after described first burst of catalyst mix;
Wherein, described degas zone is positioned at revivifier below, and regenerated catalyst enters transfer lime through standpipe, enters described external warmer under the conveying of delivery medium.
2. the method for preparing light olefins from methanol according to claim 1, is characterized in that described sial phosphorus molecular sieve comprises SAPO-34.
3. the method for preparing light olefins from methanol according to claim 1, is characterized in that described delivery medium is water vapour, comprises at least one in the hydrocarbon mixture of C4 alkene.
4. the method for preparing light olefins from methanol according to claim 1, is characterized in that in described hydrocarbon mixture, C4 alkene mass content is greater than 60%.
5. the method for preparing light olefins from methanol according to claim 1, is characterized in that described reaction zone temperature of reaction is 400~550 ℃.
6. the method for preparing light olefins from methanol according to claim 1, is characterized in that described reaction zone reaction pressure counts 0.01~0.3MPa with gauge pressure.
7. the method for preparing light olefins from methanol according to claim 1, is characterized in that described reaction zone gas phase linear speed is 0.4~3 meter per second.
8. the method for preparing light olefins from methanol according to claim 1, is characterized in that the average carbon deposition quantity massfraction of described regenerated catalyst is 0.01~0.5%.
9. the method for preparing light olefins from methanol according to claim 1, is characterized in that described isolated catalyzer is at least divided into two strands, and first strand of catalyzer accounts for 40~80% in massfraction, and second strand accounts for 20-60% in massfraction.
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Cited By (3)
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CN105669339A (en) * | 2014-11-20 | 2016-06-15 | 中国石油化工股份有限公司 | Method for preparing low carbon olefins from oxygen-containing compound by conversion |
CN110013884A (en) * | 2018-01-08 | 2019-07-16 | 神华集团有限责任公司 | Methanol-to-olefins catalyst and its preparation method and application |
CN111056893A (en) * | 2018-10-17 | 2020-04-24 | 中国石油化工股份有限公司 | Reaction system and reaction method for oxide recycling in MTO process |
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CN111056893B (en) * | 2018-10-17 | 2022-07-12 | 中国石油化工股份有限公司 | Reaction system and reaction method for recycling oxide in MTO process |
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