CN102276402B - Combined reaction apparatus for producing low-carbon olefin - Google Patents
Combined reaction apparatus for producing low-carbon olefin Download PDFInfo
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Abstract
The invention relates to a combined reaction apparatus for producing low carbon olefin. The apparatus is mainly used for solving a problem in prior arts of low low-carbon olefin yield. According to the invention, a combined reaction apparatus for producing low carbon olefin is adopted. The apparatus mainly comprises a main reaction zone 2, a first riser 13, a second riser 23, a first reclaiming zone 18, a second reclaiming zone 30, an auxiliary sedimentation zone 25, gas-solid separating equipment and catalyst circulating pipes. With the technical schemes, the problem is well solved. Therefore, the apparatus can be applied in industrialized productions of low-carbon olefin.
Description
Technical field
The present invention relates to a kind of composite reaction device of producing low-carbon alkene.
Technical background
Low-carbon alkene, ethene and propylene, be important basic chemical industry raw material, its demand is in continuous increase.Usually, ethene and propylene are to produce by petroleum path, but, due to the limited supply of petroleum resources and higher price, the cost of being produced propylene by petroleum resources constantly increases.In recent years, people start to greatly develop the technology that alternative materials transforms producing light olefins.Wherein, the important alternative materials for low-carbon alkene 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, 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 be subject to increasing attention by the technique of oxygen-containing compound conversion to produce olefine (OTO).
In the 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.The SAPO-34 catalyzer has very high selectivity of light olefin, and activity is also higher, can make the reaction times that methanol conversion is low-carbon alkene be less than the degree of 10 seconds, more even reaches in the reaction time range of riser tube.
Technology and reactor that to have announced a kind of oxygenate conversion in US6166282 be low-carbon alkene, adopt fast fluidized bed reactor, gas phase is after in gas speed, lower Mi Xiangfanyingqu has reacted, 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.Due to reaction after product gas and catalyzer sharp separation, effectively prevented the generation of secondary reaction.Through analog calculation, with traditional bubbling fluidization bed bioreactor, to compare, this fast fluidized bed reactor internal diameter and the required reserve of catalyzer all greatly reduce.But in the method, yield of light olefins is lower.
The multiple riser reaction unit of having announced in 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 in the method, yield of light olefins is lower.
Announced a kind of method that improves yield of light olefins in Chinese invention patent 200810043971.9, the first reaction zone top that it is low-carbon alkene in methanol conversion that the method adopts arranges a second reaction zone, and this second reaction zone diameter is greater than the first reaction zone, to increase the residence time of gas product in second reaction zone of the first reaction zone outlet, make unreacted methyl alcohol, the above hydrocarbon of the dme generated and carbon four continues reaction, reach the purpose that improves yield of light olefins, the method also comprises that the charging of second reaction zone can be the above hydrocarbon of freshening carbon four through separating.Although the method can improve the yield of low-carbon alkene to a certain extent, but due to the first reaction zone catalyzer out with more carbon distribution, and the above hydrocarbon pyrolysis of carbon four needs higher catalyst activity, therefore in the method, the above hydrocarbon changing effect of carbon four in second reaction zone is still on the low side, causes yield of light olefins lower.
All there is the problem that yield of light olefins is lower in prior art.The present invention has solved the problems referred to above targetedly.
Summary of the invention
Technical problem to be solved by this invention is the lower problem of yield of light olefins existed in prior art, and a kind of composite reaction device of new production low-carbon alkene is provided.This device, 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 composite reaction device of producing low-carbon alkene, mainly comprise main reaction region 2, the first riser tube 13, the second riser tube 23, the first breeding blanket 18, the second breeding blanket 30, auxiliary negative area 25, gas-solid separation equipment and catalyst recirculation pipeline etc., the first 18 tops, breeding blanket is connected with revivifier negative area 19, bottom is connected with the second breeding blanket 30, the first breeding blanket 18 is connected with the stripping zone 33 of main reactor 8 by inclined tube 6 to be generated, the first breeding blanket 18 is connected with the main reaction region 2 of main reactor 8 by regenerator sloped tube, the second 30 bottoms, breeding blanket has two catalyst outlets, with the first riser tube 13, with the second riser tube 23, be connected respectively, the first riser tube 13 is connected with auxiliary negative area 25 with the second riser tube 23 outlets, 25 bottoms, auxiliary negative area are connected with stripping zone 24, stripping zone 24 bottoms have catalyst outlet, with the first breeding blanket 18, be connected, main reactor 8, revivifier 19 and 25 tops, auxiliary negative area are equipped with pneumatic outlet.
In technique scheme, described main reaction region 2 is fast fluidized bed; Described molecular sieve comprises SAPO-34 or ZSM-5; Being equipped with gas-solid separation equipment before described pneumatic outlet, is cyclonic separator; The main reaction region charging comprises methyl alcohol, and the first riser tube 13 or the second riser tube 23 chargings are selected from the above hydrocarbon mixture of C4, ethene or petroleum naphtha; Described the first riser tube 13 and the second riser tube 23 outlets all arrange cyclonic separator; The described carbon deposition quantity of catalyst massfraction that enters the first riser tube 13 or the second riser tube 23 is less than 0.5%; Describedly from the first breeding blanket 18, return to the carbon deposition quantity of catalyst massfraction of main reaction region 2 between 0.5～2.0%; The described carbon deposition quantity of catalyst massfraction that enters the first riser tube 13 or the second riser tube 23 is less than 0.5%; Temperature of reaction in described main reaction region 2 is 400～500 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 0.8～2.0 meter per second; Temperature of reaction in the first riser tube 13 is 510～650 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 3.0～10.0 meter per seconds; Temperature of reaction in the second riser tube 23 is 500～630 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 3.0～10.0 meter per seconds; Regenerated catalyst 50～80% in described the first breeding blanket 18 enters the second breeding blanket 30, and 20-50% returns to main reaction region 2; Regenerated catalyst 30～70% in described the second breeding blanket 18 enters the first riser tube 13,30～70% and enters the second riser tube 23.
In the present invention, in main reaction region and the first riser tube, the second riser tube charging, can also add a certain amount of thinner, be selected from water vapour, the weight ratio of thinner and raw material charging is 0～1: between 1.
The inventor finds by research, and C 4 olefin or ethene can generate the low-carbon alkenes such as propylene under certain conditions.Be provided with main reaction region and assisted reaction district in the method for the invention, main reaction region is for preparing olefin by conversion of methanol, the assisted reaction district comprises the first riser tube and the second riser tube, for transforming the light hydrocarbons such as the above heavy hydrocarbon of carbon four (mixed c 4 as higher as olefin(e) centent, light naphthar etc.) or ethene, thereby reach the purpose that improves yield of light olefins.Simultaneously, because requiring of transforming of methanol conversion and heavy hydrocarbon or light hydrocarbon is different, be provided with the two-stage breeding blanket, oxygen deprivation regeneration is carried out in the first breeding blanket, be mainly main reaction region the high-selectivity catalyst with a certain amount of carbon distribution is provided, oxygen enrichment regeneration is carried out in the second breeding blanket, and for assisted reaction, district provides high activated catalyst.And the temperature of the catalyzer come from the second breeding blanket is all higher, is conducive to the above hydrocarbon of carbon four and ethene and transforms to low-carbon alkene.In addition, by the reaction in assisted reaction district, can increase the amount of burnt of revivifier, solve the lower problem of main reaction region coking yield.Therefore, adopt described method of the present invention, both can effectively improve the yield of purpose product low-carbon alkene, optimized again the energy utilization, there is process economy preferably.
Adopt technical scheme of the present invention: described main reaction region 2 is fast fluidized bed; Described molecular sieve comprises SAPO-34 or ZSM-5; Being equipped with gas-solid separation equipment before described pneumatic outlet, is cyclonic separator; The main reaction region charging comprises methyl alcohol, and the first riser tube 13 or the second riser tube 23 chargings are selected from the above hydrocarbon mixture of C4, ethene or petroleum naphtha; Described the first riser tube 13 and the second riser tube 23 outlets all arrange cyclonic separator; The described carbon deposition quantity of catalyst massfraction that enters the first riser tube 13 or the second riser tube 23 is less than 0.5%; Describedly from the first breeding blanket 18, return to the carbon deposition quantity of catalyst massfraction of main reaction region 2 between 0.5～2.0%; The described carbon deposition quantity of catalyst massfraction that enters the first riser tube 13 or the second riser tube 23 is less than 0.5%; Temperature of reaction in described main reaction region 2 is 400～500 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 0.8～2.0 meter per second; Temperature of reaction in the first riser tube 13 is 510～650 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 3.0～10.0 meter per seconds; Temperature of reaction in the second riser tube 23 is 500～630 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 3.0～10.0 meter per seconds; Regenerated catalyst 50～80% in described the first breeding blanket 18 enters the second breeding blanket 30,20～50% and returns to main reaction region 2; Regenerated catalyst 30～70% in described the second breeding blanket 18 enters the first riser tube 13,30～70% enter the second riser tube 23, in the product stream I, the low-carbon alkene carbon base absorption rate reaches 80.19% (weight), in product stream II and III, yield of light olefins reaches 48.36% (weight), has obtained technique effect preferably.
The accompanying drawing explanation
The schematic flow sheet that Fig. 1 is the method for the invention.
In Fig. 1,1 is the main reaction region bottom feed; 2 is main reaction region; 3 is the circulation inclined tube; 4 is external warmer; 5 is that in external warmer, gas returns to the main reactor pipeline; 6 is inclined tube to be generated; 7 is regenerator sloped tube; 8 is main reactor; 9 is gas-solid cyclone separator; 10 is the product stream outlet line; 11 is the first riser tube raw material charging; 12 is reclaimable catalyst lifting medium feeding line; 13 is the first riser reactor; 14 is the raising section in the reclaimable catalyst transfer line; 15 for carrying the delivery medium feeding line of regenerated catalyst to the second riser reactor; 16 is gas-solid cyclone separator; 17 is the second riser tube raw material charging; 18 is the first breeding blanket; 19 is the revivifier negative area; 20 is gas-solid cyclone separator; 21 is the regenerated flue gas outlet line; 22 for carrying the delivery medium feeding line of regenerated catalyst to the first riser reactor; 23 is the second riser reactor; 24 is stripping zone; 25 is auxiliary negative area; 26 is the product stream outlet line; 27 is stripping medium inlet pipeline; 28 is inclined tube to be generated; 29 is regenerated catalyst conveying standpipe; 30 is the second breeding blanket; 31 is the first breeding blanket regenerating medium feeding line; 32 is the second breeding blanket regenerating medium feeding line; 33 is the main reactor stripping zone.
The raw material that comprises methyl alcohol enters main reaction region 2, with the catalyzer that comprises molecular sieve, contact, generate the product stream I, form decaying catalyst simultaneously, product stream I after gas-solid separator 9 separates enters centrifugal station by outlet line 10, an isolated decaying catalyst part is returned to main reaction region 2, a part enters the first breeding blanket 18 regeneration of revivifier, one enters the second breeding blanket 30 regenerated catalyst formed, one returns to main reaction region 2, one enters the first riser tube 13 regenerated catalyst in the second breeding blanket 18, with the raw material from pipeline 11, contact, generate the product stream II, one enters second riser tube 23 in assisted reaction district, with the raw material from pipeline 17, contact, generate the product stream III, the product stream II all enters auxiliary negative area 25 with III together with catalyzer, product stream II and III after gas solid separation enter centrifugal station by pipeline 26, isolated catalyzer is back to the first breeding blanket 18 of revivifier after stripping zone 24 strippings.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
In small size back is as shown in Figure 1 answered regenerating unit, main reaction region is fast fluidized bed, revivifier arranges two-stage regeneration, the first breeding blanket is positioned at the second top, breeding blanket, the assisted reaction district arranges two riser tubes, and wherein the first riser tube top is positioned at auxiliary negative area and stripping stage inside, and the second riser tube is and assists the outside, negative area, regenerating medium is air, and the stripping medium is water vapour.The main reaction region average reaction temperature is 450 ℃, and reaction pressure is counted 0.1MPa with gauge pressure, and linear gas velocity is 1.25 meter per seconds; The first riser reactor medial temperature is 558 ℃, and reaction pressure is counted 0.1MPa with gauge pressure, and linear gas velocity is 5.0 meter per seconds; The second riser reactor medial temperature is 550 ℃, and reaction pressure is counted 0.1MPa with gauge pressure, and linear gas velocity is 5.7 meter per seconds.The main reaction region bottom feed is the methyl alcohol that purity is 99.5%, charging is 2 kg/hrs, catalyzer is SAPO-34, the first riser reactor bottom feed is mixed c 4, olefin(e) centent is 88% (weight), inlet amount is 0.54 kg/hr, the riser reaction zone bottom feed adds water vapour as thinner simultaneously, the weight ratio of water vapour and mixed c 4 is 1: 1, the second riser reactor bottom feed is the lighter hydrocarbons that the ethene mass content is 47%, wherein also comprise methane 9%, ethane 12%, propane 22%, all the other 8% are hydrogen, CO, CO
2Deng, the regenerated catalyst carbon deposition quantity massfraction that returns to main reaction region from the first breeding blanket is 1.25%, the regenerated catalyst carbon deposition quantity massfraction that enters two riser reactors from the second breeding blanket is that 0.27%, the first breeding blanket temperature is 648 ℃, and the second breeding blanket temperature is 677 ℃.The stability that keeps catalyst flow control, the reactor outlet product adopts online gas chromatographic analysis, in the product stream I, the low-carbon alkene carbon base absorption rate reaches 80.19% (weight), and in product stream II and III, yield of light olefins reaches 41.25% (weight).
[embodiment 2]
According to the described condition of embodiment 1, the main reaction region average reaction temperature is 400 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and linear gas velocity is 2.0 meter per seconds; The first riser reactor medial temperature is 510 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and linear gas velocity is 100 meter per seconds; The second riser reactor medial temperature is 500 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and linear gas velocity is 10.0 meter per seconds.The main reaction region bottom feed is the methyl alcohol that purity is 99.5%, charging is 1.74 kg/hrs, catalyzer is SAPO-34, the first riser reactor bottom feed is mixed c 4, olefin(e) centent is 88% (weight), inlet amount is 0.24 kg/hr, the riser reaction zone bottom feed adds water vapour as thinner simultaneously, the weight ratio of water vapour and mixed c 4 is 1: 1, the second riser reactor bottom feed is the lighter hydrocarbons that the ethene mass content is 47%, wherein also comprise methane 9%, ethane 12%, propane 22%, all the other 8% are hydrogen, CO, CO
2Deng, the regenerated catalyst carbon deposition quantity massfraction that returns to main reaction region from the first breeding blanket is 0.5%, the regenerated catalyst carbon deposition quantity massfraction that enters two riser reactors from the second breeding blanket is 0.16%, the stability that keeps catalyst flow control, the reactor outlet product adopts online gas chromatographic analysis, in the product stream I, the low-carbon alkene carbon base absorption rate reaches 77.97% (weight), and in product stream II and III, yield of light olefins reaches 38.45% (weight).
[embodiment 3]
According to the described condition of embodiment 1, the main reaction region average reaction temperature is 500 ℃, and reaction pressure is counted 0.3MPa with gauge pressure, and linear gas velocity is 0.8 meter per second; The first riser reactor medial temperature is 650 ℃, and reaction pressure is counted 0.3MPa with gauge pressure, and linear gas velocity is 3.0 meter per seconds; The second riser reactor medial temperature is 630 ℃, and reaction pressure is counted 0.3MPa with gauge pressure, and linear gas velocity is 3.0 meter per seconds.The main reaction region bottom feed is the methyl alcohol that purity is 99.5%, charging is 2.96 kg/hrs, catalyzer is SAPO-34, the first riser reactor bottom feed is mixed c 4, olefin(e) centent is 61% (weight), inlet amount is 0.67 kg/hr, the riser reaction zone bottom feed adds water vapour as thinner simultaneously, the weight ratio of water vapour and mixed c 4 is 1: 1, the second riser reactor bottom feed is the lighter hydrocarbons that the ethene mass content is 31%, wherein also comprise methane 10.2%, ethane 18%, propane 27%, all the other 13.8% are hydrogen, CO, CO
2Deng, the regenerated catalyst carbon deposition quantity massfraction that returns to main reaction region from the first breeding blanket is 2.0%, the regenerated catalyst carbon deposition quantity massfraction that enters two riser reactors from the second breeding blanket is 0.5%, the stability that keeps catalyst flow control, the reactor outlet product adopts online gas chromatographic analysis, in the product stream I, the low-carbon alkene carbon base absorption rate reaches 7628% (weight), and in product stream II and III, yield of light olefins reaches 35.22% (weight).
[embodiment 4]
In small size back is as shown in Figure 1 answered regenerating unit, the main reaction region average reaction temperature is 425 ℃, and the first riser reactor medial temperature is 610 ℃, and the second riser reactor medial temperature is 610 ℃.Catalyzer is ZSM-5, and the first riser reactor bottom feed is light naphthar, forms in Table 1.The riser reaction zone bottom feed adds water vapour as thinner simultaneously, the weight ratio of water vapour and mixed c 4 is 1: 1, the second riser reactor bottom feed is that olefin(e) centent is at carbon four～carbon six hydrocarbon mixtures more than 70% (wherein carbon four hydrocarbon total mass marks are more than 85%), the regenerated catalyst carbon deposition quantity massfraction that enters two riser reactors from the second breeding blanket is 0.16%, the stability that keeps catalyst flow control, the reactor outlet product adopts online gas chromatographic analysis, in the product stream I, the low-carbon alkene carbon base absorption rate reaches 67.25% (weight), in product stream II and III, yield of light olefins reaches 48.36% (weight).
Table 1 light naphthar forms distribution
| Initial boiling point, ℃ | 40 |
| Final boiling point, ℃ | 162 |
| Alkane, % by weight | 65.18 |
| Normal paraffin, % by weight | 32.54 |
| Alkene, % by weight | 0.17 |
| Naphthenic hydrocarbon, % by weight | 28.44 |
| Aromatic hydrocarbons, % by weight | 6.21 |
Obviously, adopt method of the present invention, can reach the purpose that improves yield of light olefins, there is larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (5)
1. a composite reaction device of producing low-carbon alkene, mainly comprise main reaction region (2), the first riser tube (13), the second riser tube (23), the first breeding blanket (18), the second breeding blanket (30), auxiliary negative area (25), gas-solid separation equipment and catalyst recirculation pipeline etc., top, the first breeding blanket (18) is connected with revivifier negative area (19), bottom is connected with the second breeding blanket (30), the first breeding blanket (18) is connected with the stripping zone (33) of main reactor (8) by inclined tube to be generated (6), the first breeding blanket (18) is connected with the main reaction region (2) of main reactor (8) by regenerator sloped tube, bottom, the second breeding blanket (30) has two catalyst outlets, with the first riser tube (13), with the second riser tube (23), be connected respectively, with the second riser tube (23), outlet is connected with auxiliary negative area (25) the first riser tube (13), bottom, auxiliary negative area (25) is connected with stripping zone (24), stripping zone (24) bottom has catalyst outlet, with the first breeding blanket (18), be connected, main reactor (8), revivifier (19) and top, auxiliary negative area (25) are equipped with pneumatic outlet,
The described carbon deposition quantity of catalyst massfraction that enters the first riser tube (13) or the second riser tube (23) is less than 0.5%; Describedly from the first breeding blanket (18), return to the carbon deposition quantity of catalyst massfraction of main reaction region (2) between 0.5～2.0%;
Described main reaction region charging comprises methyl alcohol, and the first riser tube (13) or the second riser tube (23) charging are selected from the above hydrocarbon mixture of C4, ethene or petroleum naphtha.
2. produce according to claim 1 the composite reaction device of low-carbon alkene, it is characterized in that described main reaction region (2) is for fast fluidized bed; Described molecular sieve comprises SAPO-34 or ZSM-5.
3. producing according to claim 1 the composite reaction device of low-carbon alkene, it is characterized in that being equipped with gas-solid separation equipment before described pneumatic outlet, is cyclonic separator.
4. produce according to claim 1 the composite reaction device of low-carbon alkene, it is characterized in that described the first riser tube (13) and the second riser tube (23) outlet all arrange cyclonic separator.
5. produce according to claim 1 the composite reaction device of low-carbon alkene, it is characterized in that the temperature of reaction in described main reaction region (2) is 400～500 ℃, reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 0.8～2.0 meter per second; Temperature of reaction in the first riser tube (13) is 510～650 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 3.0～10.0 meter per seconds; Temperature of reaction in the second riser tube (23) is 500～630 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 3.0～10.0 meter per seconds.
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| CN103539611B (en) * | 2012-07-09 | 2016-06-08 | 中国石油化工集团公司 | A kind of device utilizing oxygenatedchemicals producing olefinic hydrocarbons |
| CN103539616B (en) * | 2012-07-09 | 2016-08-03 | 中国石油化工集团公司 | A kind of oxygenatedchemicals olefins process |
| CN103539610B (en) * | 2012-07-09 | 2016-06-08 | 中国石油化工集团公司 | A kind of oxygenatedchemicals produces olefin hydrocarbon apparatus |
| CN103539598B (en) * | 2012-07-09 | 2016-06-08 | 中国石油化工集团公司 | A kind of oxygenatedchemicals produces the method for low-carbon alkene |
| CN103739429B (en) * | 2012-10-17 | 2016-05-18 | 中国石油化工股份有限公司 | The reaction unit of preparing light olefins from methanol |
| CN103772091B (en) * | 2012-10-25 | 2016-04-13 | 中国石油化工股份有限公司 | By the method for preparing low carbon olefin hydrocarbon with methanol |
| CN107540498A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | By methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene |
| CN107540496A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | Methanol or the method for dimethyl ether production aromatic hydrocarbons and low-carbon alkene |
| CN107540492A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | By methanol or the method for dimethyl ether production aromatic hydrocarbons and low-carbon alkene |
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| CN102276402A (en) | 2011-12-14 |
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