CN102276379B - Method for coproducing dimethyl ether serving as byproduct in process of preparing low-carbon olefin through methanol conversion - Google Patents
Method for coproducing dimethyl ether serving as byproduct in process of preparing low-carbon olefin through methanol conversion Download PDFInfo
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- CN102276379B CN102276379B CN201010199695.2A CN201010199695A CN102276379B CN 102276379 B CN102276379 B CN 102276379B CN 201010199695 A CN201010199695 A CN 201010199695A CN 102276379 B CN102276379 B CN 102276379B
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Abstract
The invention relates to a method for coproducing dimethyl ether serving as a byproduct in a process of preparing low-carbon olefin through methanol conversion, and the method can be mainly used for solving the problem of single catalyst system during dimethyl ether production in the prior art. The method for coproducing dimethyl ether serving as the byproduct in the process of preparing low-carbon olefin through methanol conversion mainly comprises the following steps of: a, enabling a raw material comprising methanol to be in contact with molecular sieve based catalysts in a first reactor to generate a product material flow I comprising low-carbon olefin; b, carrying out gas-solid separation on a carbon deposit catalyst carried in the material flow I to form a coked catalyst to enter a precipitator, wherein the coked catalyst in the precipitator is divided into at least three parts, the first part enters a second reactor through a rapid bed pipeline, the second part returns to the first reactor through a circulating pipeline, the third part enters a regenerator through a pending pipeline; c, enabling the raw material comprising the methanol to be in contact with the coked catalyst in the second reactor to generate a product material flow II comprising dimethyl ether, carrying out gas-solid separation on a catalyst carried in the material flow II to enter the precipitator, mixing the material flow II into the material flow I and flowing out of the precipitator; and d, carrying out regenerating on the carbon deposit catalyst through the regenerator and steam stripping on the carbon deposit catalyst through a steam stripper, and then enabling the carbon deposit catalyst to enter the first reactor through a regeneration pipeline. According to the technical scheme, the problem is better solved, thus the method provided by the invention can be used in industrial production for producing the low-carbon olefin through methanol conversion.
Description
Technical field
The present invention relates to a kind of method of methanol-to-olefins reaction byproduct in process dme.
Background technology
Low-carbon alkene, is defined as ethene and propylene here, is two kinds of important basic chemical industry raw materials, and its demand is in continuous increase.Ethene, propylene are mainly to make by petroleum path traditionally, 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 substitute energy transformation technology, and as the technique of oxygen-containing compound conversion to produce olefine (OTO), oxygenatedchemicals comprises methyl alcohol, ethanol, dme, methyl ethyl ether, methylcarbonate etc.Have many technology to can be used to produce oxygenatedchemicals, raw material comprises coal, Sweet natural gas, biomass etc.As methyl alcohol, can be made by coal or Sweet natural gas, technique is very ripe, can realize the industrial scale of up to a million tonnes.Popularity due to 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), particularly the technique by preparing olefin by conversion of methanol (MTO) is subject to increasing attention.
Dme (DME) is as a kind of emerging basic chemical raw materials, and excellent performance, has the advantages such as burning highly effective, cleaning, safety as domestic fuel and automobile fuel, is the desirable alternative fuel of diesel oil and liquefied petroleum gas (LPG).Can be used as the propellent of aerosol, substitute Chlorofluorocarbons (CFCs) (fluorine Lyons), liquefaction third (fourth) alkane gas, become the 4th generation propellent main body.Dme is also important industrial chemicals, at medicine, agricultural chemicals and dyestuffs industries, is widely used.
In CN1962594A patent, adopt fluid bed reactor methanol gas phase dehydration preparing dimethy ether, catalyzer adopts gama-alumina, and reaction conversion ratio reaches 89%, and selectivity is greater than 99%, and fluidized-bed inner catalyst upgrades, regeneration is easy, can keep catalyst activity stable.But this process design is unreasonable, and temperature of reaction is higher.
For MTO technology, on SAPO-34 catalyzer, long-pending a certain amount of carbon can effectively improve the selectivity of low-carbon alkene in reaction product, and has a best catalyst carbon deposit weight range to make in product the selectivity of low-carbon alkene the highest.Current methanol-to-olefins method, on catalyst surface, control and adhere to certain coke content, effectively improved the selectivity of low-carbon alkene in product, the meanwhile also corresponding raising with the increase of coke content of the selectivity of dme in product, along with catalyzer coke content further increases, the selectivity of dme increases substantially, and therefore, needs independent separating device to isolate dme a small amount of in product.
Summary of the invention
Technical problem to be solved by this invention is that in prior art, dme is produced the single problem of catalyst system, and the method for by-product dme in a kind of new preparing light olefins from methanol is provided.The method, for the production of low-carbon alkene, has advantages of and can utilize the carbon deposited catalyst of preparing olefin by conversion of methanol to produce dme, raising dme output.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method of methanol-to-olefins reaction byproduct in process dme, mainly comprise the following steps: a) raw material that comprises methyl alcohol is contacted in the first reactor with molecular sieve catalyst, generate the product logistics I that comprises low-carbon alkene; B) carbon deposited catalyst that logistics I is carried secretly forms spent agent and enters settling vessel after gas solid separation, in settling vessel, spent agent is at least divided into three parts, first part enters the second reactor through fast bed pipeline, second section returns to the first reactor through circulation line, and third part enters revivifier through pipeline to be generated; C) raw material containing methyl alcohol contacts in the second reactor with spent agent, generates the product logistics II that comprises dme, and the catalyzer that logistics II is carried secretly enters settling vessel after gas solid separation, and logistics II flows out settling vessel after being incorporated to logistics I; D) carbon deposited catalyst, after revivifier regeneration, stripper stripping, enters the first reactor through regeneration pipeline.
In technique scheme, the first reactor fast fluidized bed reactor, the second reactor is riser reactor, and molecular sieve catalyst comprises and is selected from SAPO-5, SAPO-11, SAPO-18, SAPO-20, SAPO-34, SAPO-44 or SAPO-56 silicoaluminophosphamolecular molecular sieve catalyst; The temperature of reaction of the first reactor is 350～600 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 0.8～2.5 meter per second; The temperature of reaction of the second reactor is 200～420 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 3.0～10.0 meter per seconds.Molecular sieve catalyst is selected from SAPO-34 silicoaluminophosphamolecular molecular sieve catalyst; The temperature of reaction of the first reactor is preferably 400～500 ℃, and reaction pressure is preferably 0.1～0.2MPa in gauge pressure, and linear gas velocity is preferably 1.0～1.5 meter per seconds; The temperature of reaction of the second reactor is preferably 320～380 ℃, and reaction pressure is preferably 0.1～0.2MPa in gauge pressure, and linear gas velocity is preferably 5.0～8.0 meter per seconds.Spent agent is in mass flux ratio first part in settling vessel: second section: third part=0.01～10: 1: 0.01～10.Spent agent is in the preferred first part of mass flux ratio in settling vessel: second section: third part=0.05～1: 1: 0.05～1.Temperature in revivifier is between 550～700 ℃, in revivifier, take gauge pressure pressure as 0～1MPa.Temperature in revivifier is preferably 600～650 ℃, in revivifier, in gauge pressure pressure, is preferably 0.1～0.3MPa.The average coke content of settling vessel inner catalyst is 1～9%.The average coke content of settling vessel inner catalyst is preferably 2～6%.
Adopt method of the present invention, in settling vessel, the carbon deposition catalyst of inactivation is sent into riser tube and methanol mixed, reaction is removed separation circuit after generating and mixing containing the product of dme and the product of methanol-to-olefins, can effectively improve the output of methanol-to-olefins by product dme.Therefore, method of the present invention can effectively utilize the spent agent in methanol to olefins reaction to prepare dme, makes full use of dme separating device effective output that increases dme, and easy to operate, is easy to control.
Adopt technical scheme of the present invention: the first reactor fast fluidized bed reactor, the second reactor is riser reactor, and molecular sieve catalyst comprises silicoaluminophosphamolecular molecular sieve catalysts such as being selected from SAPO-5, SAPO-11, SAPO-18, SAPO-20, SAPO-34, SAPO-44, SAPO-56.The temperature of reaction of the first reactor is 350～600 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 0.8～2.5 meter per second; The temperature of reaction of the second reactor is 200～420 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and linear gas velocity is 3.0～10.0 meter per seconds.Spent agent is in mass flux ratio first part in settling vessel: second section: third part=0.01～10: 1: 0.01～10.Temperature in revivifier is between 550～700 ℃, in revivifier, take gauge pressure pressure as 0～1MPa.The average coke content of settling vessel inner catalyst is 1～9%.In product, ethene+propylene carbon base absorption rate can reach 63.43% weight, and the yield of dme can reach 19.29% weight simultaneously, has 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 settling vessel; 2 is the second reactor; 3 is fast bed pipeline; 4 is circulation line; 5 is material benzenemethanol; 6 is the first reactor; 7 is revivifier; 8 is stripper; 9 is regeneration pipeline; 10 is pipeline to be generated.
Material benzenemethanol 5 enters reactor from the first reactor 6 bottoms, contact and react with the catalyzer of catalyst recycle line 4, gas-solid mixture enters the catalyst settler 1 of reaction unit after sharp separation, and the interior gaseous products of settling vessel 1 enters follow-up centrifugal station after cyclonic separator is deviate from catalyzer.Spent agent in settling vessel is divided into three parts, and first part's catalyzer enters the second reactor 2 through fast bed pipeline 3 and contacts with methyl alcohol 5, and its product and catalyzer enter settling vessel 1 after gas solid separation; Second section catalyzer returns to the first reactor 6 through circulation line 4; Third part enters revivifier 7 through pipeline 10 to be generated, and the carbon deposited catalyst that enters revivifier 7 enters stripper 8 after contacting with regenerating medium and burning, and the regenerated catalyst after stripping is delivered to the first reactor 6 through regeneration pipeline 9.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1～4]
On reaction unit as shown in Figure 1, raw material is methyl alcohol, and the first reactor adopts fast fluidized bed, and the second reactor is riser tube, and temperature of reaction is 450 ℃, and in reactor, linear gas velocity is 1.5 meter per seconds; Riser temperature is 320 ℃, in riser tube, linear gas velocity is 8.0 meter per seconds, reactor, riser tube and revivifier pressure are 0.01MPa in gauge pressure, revivifier adopts fluidized-bed, regenerating medium is air, regeneration temperature is 650 ℃, and the thief hole of spent agent is positioned at pipeline 10 to be generated, and on catalyzer, the analysis of carbon content adopts Infrared Carbon-sulphur high speed analysis instrument.The coke content of controlling reclaimable catalyst is 5.9% (weight percent), the mass rate of reclaimable catalyst three parts is remained on to quick pipeline flow: circulation line flow: pipeline to be generated flow=0.1: 1: 0.1, make system run all right, control conveniently.Catalyzer adopts respectively SAPO-34, SAPO-11, SAPO-18, the SAPO-56 molecular sieve catalyst of spray-dried moulding.Reactor outlet product adopts online gas chromatographic analysis, and experimental result is in Table 1.
Table 1
| Parameter | Catalyst type | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Yield of dimethyl ether, % (weight) |
| Embodiment 1 | SAPO-34 | 34.50 | 27.39 | 19.94 |
| Embodiment 2 | SAPO-11 | 6.81 | 18.49 | 25.61 |
| Embodiment 3 | SAPO-18 | 32.61 | 22.67 | 18.21 |
| Embodiment 4 | SAPO-56 | 22.91 | 18.14 | 20.45 |
[embodiment 5～8]
According to the condition described in embodiment 1, just change the temperature of the first reactor, experimental result is in Table 2.
Table 2
| Parameter | The first temperature of reactor ℃ | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Yield of dimethyl ether, % (weight) |
| Embodiment 5 | 350 | 20.23 | 21.25 | 23.09 |
| Embodiment 6 | 400 | 32.49 | 27.28 | 20.18 |
| Embodiment 7 | 500 | 36.99 | 24.49 | 19.45 |
| Embodiment 8 | 600 | 42.14 | 16.58 | 18.82 |
[embodiment 9～11]
According to the condition described in embodiment 1, just change the temperature of reaction of the second reactor, experimental result is in Table 3.
Table 3
| Parameter | Riser temperature ℃ | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Yield of dimethyl ether, % (weight) |
| |
200 | 34.35 | 27.41 | 10.78 |
| Embodiment 10 | 380 | 35.27 | 27.28 | 16.91 |
| Embodiment 11 | 420 | 35.67 | 27.88 | 11.51 |
[embodiment 12～14]
Condition according to described in embodiment 1, just changes reactor linear speed, and experimental result is in Table 4.
Table 4
| Parameter | Reactor linear speed, meter per second | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Yield of dimethyl ether, % (weight) |
| Embodiment 12 | 0.8 | 30.22 | 20.15 | 19.21 |
| Embodiment 13 | 1.0 | 35.02 | 28.41 | 19.29 |
| Embodiment 14 | 2.5 | 32.01 | 22.72 | 20.11 |
[embodiment 15～17]
Condition according to described in embodiment 1, just changes riser tube linear speed, and experimental result is in Table 5.
Table 5
| Parameter | Riser tube linear speed, meter per second | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Yield of dimethyl ether, % (weight) |
| Embodiment 15 | 3.0 | 34.40 | 27.29 | 20.81 |
| Embodiment 16 | 5.0 | 34.45 | 26.33 | 19.99 |
| Embodiment 17 | 10 | 34.49 | 26.38 | 10.08 |
[embodiment 18～22]
According to the condition described in embodiment 1, just change the ratio of the mass rate of reclaimable catalyst three parts, experimental result is in Table 6.
Table 6
| Parameter | Quick pipeline: circulation line: pipeline to be generated (mass flux ratio) | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Yield of dimethyl ether, % (weight) |
| Embodiment 18 | 0.05∶1∶0.1 | 35.21 | 27.88 | 5.27 |
| Embodiment 19 | 1∶1∶0.1 | 33.13 | 26.20 | 15.01 |
| Embodiment 20 | 0.1∶1∶0.05 | 29.76 | 25.31 | 11.98 |
| Embodiment 21 | 0.1∶1∶1 | 34.53 | 27.42 | 18.12 |
| Embodiment 22 | 1∶1∶0.05 | 26.23 | 23.94 | 7.09 |
[embodiment 23～25]
Condition according to described in embodiment 1, just changes regenerator temperature, and experimental result is in Table 7.
Table 7
| Parameter | Regeneration temperature, ℃ | Regenerator coke content, % (weight) | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Yield of dimethyl ether, % (weight) |
| Embodiment 23 | 550 | 1.41 | 34.37 | 26.81 | 20.45 |
| Embodiment 24 | 600 | 1.04 | 34.73 | 27.44 | 20.08 |
| Embodiment 25 | 700 | 0.01 | 34.11 | 27.55 | 19.91 |
[embodiment 26～28]
According to the condition described in embodiment 1, reactor, riser tube and revivifier adopt same press operation, change the pressure of reactor, riser tube and revivifier, and experimental result is in Table 8.
Table 8
| Parameter | The pressure of reaction-regeneration system, MPa | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Yield of dimethyl ether, % (weight) |
| Embodiment 26 | 0.1 | 33.48 | 26.94 | 20.29 |
| Embodiment 27 | 0.2 | 32.51 | 26.16 | 20.77 |
| Embodiment 28 | 0.3 | 27.81 | 23.35 | 21.22 |
[embodiment 29～32]
According to the condition described in embodiment 1, just change the coke content of reclaimable catalyst, experimental result is in Table 9.
Table 9
| Parameter | Spent agent coke content, % (weight) | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Yield of dimethyl ether, % (weight) |
| Embodiment 29 | 1.00 | 31.22 | 28.37 | 23.32 |
| Embodiment 30 | 2.05 | 32.68 | 28.01 | 20.97 |
| Embodiment 31 | 7.50 | 30.27 | 20.91 | 15.45 |
| Embodiment 32 | 9.20 | 28.70 | 16.09 | 12.62 |
Obviously, adopt method of the present invention, can effectively utilize the spent agent in methanol to olefins reaction to prepare dme, effectively increase the output of dme, improved the utilization ratio of dme separating device, and easy to operate, be easy to control, can be used in the industrial production of low-carbon alkene.
Claims (1)
1. the method for a methanol-to-olefins reaction byproduct in process dme, material benzenemethanol (5) enters reactor from the first reactor (6) bottom, the catalyzer coming with catalyst recycle line (4) contacts and reacts, gas-solid mixture enters the catalyst settler (1) of reaction unit after sharp separation, and the interior gaseous products of settling vessel (1) enters follow-up centrifugal station after cyclonic separator is deviate from catalyzer; Spent agent in settling vessel is divided into three parts, and first part's catalyzer enters the second reactor (2) through fast bed pipeline (3) and contacts with methyl alcohol (5), and its product and catalyzer enter settling vessel (1) after gas solid separation; Second section catalyzer returns to the first reactor (6) through circulation line (4); Third part enters revivifier (7) through pipeline to be generated (10), the carbon deposited catalyst that enters revivifier (7) enters stripper (8) after contacting with regenerating medium and burning, and the regenerated catalyst after stripping is delivered to the first reactor (6) through regeneration pipeline (9);
Wherein, raw material is methyl alcohol, and the first reactor adopts fast fluidized bed, and the second reactor is riser tube, and temperature of reaction is 450 ℃, and in reactor, linear gas velocity is 1.0 meter per seconds; Riser temperature is 320 ℃, in riser tube, linear gas velocity is 8.0 meter per seconds, reactor, riser tube and revivifier pressure are 0.01MPa in gauge pressure, revivifier adopts fluidized-bed, regenerating medium is air, regeneration temperature is 650 ℃, and the thief hole of spent agent is positioned at pipeline to be generated (10), and on catalyzer, the analysis of carbon content adopts Infrared Carbon-sulphur high speed analysis instrument; Control the coke content of reclaimable catalyst, be 5.9% by weight percentage, the mass rate of reclaimable catalyst three parts is remained on to quick pipeline flow: circulation line flow: pipeline to be generated flow=0.1: 1: 0.1, catalyzer adopted the SAPO-34 of spray-dried moulding; Reactor outlet product adopts online gas chromatographic analysis, and result is, by weight percentage, ethene carbon base absorption rate 35.02%, propylene carbon base absorption rate 28.41%, yield of dimethyl ether is 19.29%.
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