CN101555193A - Separating method of aqueous phase byproduct from Fischer-Tropsch synthesis - Google Patents
Separating method of aqueous phase byproduct from Fischer-Tropsch synthesis Download PDFInfo
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- CN101555193A CN101555193A CNA2008100432527A CN200810043252A CN101555193A CN 101555193 A CN101555193 A CN 101555193A CN A2008100432527 A CNA2008100432527 A CN A2008100432527A CN 200810043252 A CN200810043252 A CN 200810043252A CN 101555193 A CN101555193 A CN 101555193A
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Abstract
The invention relates to a separating method of an aqueous phase byproduct from Fischer-Tropsch synthesis and mainly aims at solving the problem that the direct discharge of the aqueous phase byproduct of Fischer-Tropsch synthesis at present is not economical and pollutes the environment. The method adopts the following steps: the aqueous phase byproduct enters the middle part of a common rectifying tower 1, a distillate stream I with the boiling range of 50-120 DEG C is extracted at a lateral line, a light component with a boiling range of less than 40 DEG C is obtained at the top of the tower, and a heavy component with the boiling range of more than 120 DEG C is obtained at a kettle of the tower; and the lateral line distillate is rectified and separated by an isolating tower 2, a co-boiling rectifying tower 3, an acetic acid extraction tower 4 and an extractant recovering tower 5 so as to obtain methanol-acetone solution, ethanol, n-propanol and a basic organic raw material of acetic acid, and such a technical scheme better solves the problem and can be used in the industrial production for treating the aqueous phase byproduct from the Fischer-Tropsch synthesis.
Description
Technical field
The present invention relates to a kind of separation method of aqueous phase by-product of fischer-tropsch synthesis reaction.
Background technology
Along with based on the increase of the liquid fuel demand of oil and the minimizing of petroleum resources usable reserves, the method for being produced the available liquid fuel by solid fuels such as coals more and more is subject to people's attention.Solid-fuelled liquefaction has two kinds of different technological lines, and a kind of is direct liquefaction, and a kind of is indirect liquefaction.Direct liquefaction is under High Temperature High Pressure, solid fuels such as coal is converted into the technology of liquefaction oil under the effect of solvent and catalyzer.Direct liquefaction operational condition harshness is strong to the dependency of raw material.Indirect liquefaction is that the Fischer-Tropsch of common indication is synthetic, be at iron-based, bore under the condition of base or the catalyst based existence of anvil, the synthetic gas that comprises carbon monoxide and hydrogen that will produce by solid fuels such as coals, under certain temperature and pressure, the technology of directional catalyzing synthin fuel and industrial chemicals.Indirect liquefaction is strong to the suitability of raw material, and range of product is many, institute's produce oil product quality height.
Fischer-Tropsch synthetic raw material is the synthetic gas based on carbon monoxide and hydrogen, and synthetic gas is to be obtained by solid fuel gasifications such as coals.Need before the solid fuel gasification to mix to roll with water earlier to make slurry.Mainly be carbon monoxide and hydrogen generate methane and higher carbon number under the catalyst based effect of iron-based, brill base or anvil hydro carbons in the fischer-tropsch reaction process, generate alcohol, other hydrocarbon oxide and reaction water simultaneously.
Reaction water can be separated easily with Fischer-Tropsch synthetic principal product hydrocarbon, but because hydrocarbon oxides such as alcohol have certain solubleness in water, so isolated reaction water contains organic oxygen-containing compounds such as certain alcohol, aldehyde, ketone and acid from Fischer-Tropsch synthetic.
Because the amount of the reaction water that generates in the Fischer-Tropsch building-up process is bigger, it is emitted, obviously be uneconomic, and, can cause corrosion and pollution that directly discharging does not meet environmental requirement yet owing to contain organic oxygen-containing compounds such as alcohol, aldehyde, ketone and acid in the reaction water.Introduced the separation of aqueous phase by-product of fischer-tropsch synthesis reaction among the patent CN 1696082A simply, aqueous phase by-product is separated into the mixture and the reaction water that contains the higher organic oxygen-containing compound of boiling point of the light constituent oxygenatedchemicalss such as alcohol ketone that contain less water by conventional distillation, the overhead mixture use that acts as a fuel, tower still reaction water loops back the synthetic gas stage, makes slurry with solid mixtures such as coals.This patent is just handled aqueous phase by-product from environmental angle, does not make full use of each basic organic in the aqueous phase by-product, and the whole separation process of explanation aqueous phase by-product.
Summary of the invention
Technical problem to be solved by this invention is the directly uneconomical and problem of environment pollution caused of discharging of present aqueous phase by-product of fischer-tropsch synthesis reaction, and a kind of method of separating aqueous phase byproduct from Fischer-Tropsch synthesis reaction is provided.This method has simple, the cost-effective characteristics of flow process.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of separation method of aqueous phase by-product of fischer-tropsch synthesis reaction, may further comprise the steps: a) aqueous phase by-product enters the middle part of common rectifying tower 1, the cut stream I that the side line extraction is 50～120 ℃, cat head obtains boiling point less than 40 ℃ light constituent, and the tower still obtains boiling point greater than 120 ℃ heavy constituent; B) stream I enters the middle part of separating tower 2 left sides, and overhead distillate is methyl alcohol, acetone soln stream I I, and the tower still obtains aqueous acetic acid stream I II, side line extraction ethanol on the right side, following side line extraction n-propyl alcohol aqueous solution stream I V; C) stream I II enters the middle part of azeotropy rectification column 3, water extraction in the cat head phase splitter, and oil phase refluxes, and the discharging of tower still is a n-propyl alcohol, and wherein entrainer is selected from water and forms at least a in the minimum azeotropic mixture; D) stream I I enters the cat head of acetic acid extraction tower 4, and acetic acid extraction tower cat head obtains acetic acid, extractant mixture stream I V, and the tower still is a waste water, and wherein extraction agent is selected from least a in organic phosphine or the organic amine; E) stream I V enters the middle part of extraction agent recovery tower 5, and overhead distillate is an acetic acid, and the tower still obtains reclaiming extraction agent.
In technique scheme, the theoretical plate number of common rectifying tower 1 is 10～60, and reflux ratio is 1～12, and tower top temperature control is not less than 40 ℃; The theoretical plate number of azeotropy rectification column 3 is 15～60, and entrainer and raw material ratio are 0.2～1, and control tower still temperature is 96.8～97.5 ℃; The theoretical plate number of acetic acid extraction tower 4 is 10～40, and extraction agent and raw material ratio are 1～6, normal-temperature operation; The theoretical plate number of extraction agent recovery tower 5 is 10～50, and reflux ratio is 1～6, decompression operation; The theoretical plate number of separating tower 2 is 50～200, division plate top accounts for 1/6～1/3 theoretical stage, the division plate bottom accounts for 1/6～1/3 theoretical stage, the left side liquid phase distribution mark on division plate top is 0.3～0.7, the left side gas phase distribution mark of division plate bottom is 0.3～0.7, and reflux ratio is 5～30, and tower top temperature is controlled to be 60～64 ℃, last side line extraction temperature is controlled to be 68～68.5 ℃, and following side line extraction temperature is controlled to be 87～93 ℃; Azeotropy rectification column 3 used entrainers are at least a in hexanaphthene, Iso Butyl Acetate or n-butyl acetate preferably; Acetic acid extraction tower 4 used extraction agents are at least a in trialkyl phosphine or TERTIARY BUTYL AMINE preferably.
Because the component complexity of aqueous phase by-product of fischer-tropsch synthesis reaction can adopt the method for conventional distillation to remove a spot of light and heavy component, the side line extraction obtains a large amount of intermediate component.The content of water accounts for more than 80% of weight composition in the intermediate component, consider from saving the energy consumption aspect, most of water is removed from cutting apart the Tata still as heavy key, cat head obtains acetone and methanol solution, top side line extraction ethanol, the bottom side line extraction n-propyl alcohol aqueous solution, the aqueous acetic acid that acetic acid cutting Tata still obtains can be by extraction with acetic acid and water sepn, and the n-propyl alcohol aqueous solution adopts azeotropic distillation to separate.By adopting the technical scheme of common rectifying tower, splitter, azeotropy rectification column, acetic acid extraction tower, extraction agent recovery tower five tower flow processs, make aqueous phase by-product of fischer-tropsch synthesis reaction be separated, obtained better technical effect.
Description of drawings
Fig. 1 is for separating the flow process of aqueous phase byproduct from Fischer-Tropsch synthesis.
1 is common rectifying tower among Fig. 1, and 2 for separating tower, and 3 is azeotropy rectification column, and 4 is the acetic acid extraction tower, 5 is the extraction agent recovery tower, and 6 is aqueous phase by-product, and 7 is light constituent, and 9 are heavy constituent, 8 is side stream, and 10 is methyl alcohol and acetone soln, and 11 is ethanol, 12 is the n-propyl alcohol aqueous solution, and 13 is aqueous acetic acid, and 14 is extraction agent, 15 is azeotropic water, and 16 is n-propyl alcohol, and 17 is acetic acid, extractant mixture, 18 is waste water, and 19 is acetic acid, and 20 for reclaiming extraction agent.
By flow process shown in Figure 1, aqueous phase by-product 6 enters the middle part of common rectifying tower 1, and cat head distillates and is light component 7, Tower reactor obtains restructuring and divides 9, and the side line extraction is side run-off 8, and side run-off 8 enters the left side central portion of separating tower 2, cat head Distillate and be acetone and methanol solution 10, tower reactor obtains aqueous acetic acid 13, and the top side line extraction on right side is ethanol 11, the right side The bottom side line extraction of side is the normal propyl alcohol aqueous solution 12, and the normal propyl alcohol aqueous solution 12 enters the middle part of azeotropy rectification column 3, cat head Water extraction azeotropic water 15, tower reactor obtains normal propyl alcohol 16, and aqueous acetic acid 13, extractant 14 are respectively from Extraction of Acetic Acid tower 4 Top, bottom enter, cat head distillates and is acetic acid, extractant mixture 17, tower reactor is waste water 18, acetic acid, extractant Mixture 17 enters the middle part of extractant recovery tower 5, and cat head distillates and is acetic acid 19, and tower reactor obtains reclaiming extractant 20.
The present invention is further illustrated below by specific embodiment, and still, scope of the present invention has more than and is limited to enforcement The scope that example covers.
Embodiment
[embodiment 1]
By flow process shown in Figure 1, (boiling point is less than 40 ℃ component for aqueous phase byproduct from Fischer-Tropsch synthesis 6, boiling range be 50～120 ℃ component and boiling point greater than 120 ℃ component account for respectively that weight forms 5%, 85% and 10%) entering number of theoretical plate is 15 common rectifying tower 1, feed entrance point is the 7th a block of theoretical tray, reflux ratio is 12, the control tower top temperature is 40 ℃, it from the 8th theoretical tray side line extraction boiling range 50～120 ℃ cut 8, it is 50 separation tower 2 that side stream 8 enters number of theoretical plate, the number of theoretical plate on division plate top is 10, the bottom number of theoretical plate also is 10, the liquid phase distribution mark of division plate upper left-hand is 0.7, the gas phase distribution mark of lower left side is 0.68, reflux ratio is 30, tower top temperature is controlled to be 60～64 ℃, last side line extraction temperature is controlled to be 68～68.5 ℃, following side line extraction temperature is controlled to be 87～93 ℃, overhead fraction is acetone and carbinol mixture 10, separating tower top side line extraction is ethanol 11, separating the tower bottom side line extraction n-propyl alcohol aqueous solution 12, to enter theoretical plate number be 20 azeotropy rectification column 3, feed entrance point is the 12nd a block of theoretical tray, entrainer is selected hexanaphthene for use, entrainer and raw material ratio are 0.9, control tower still temperature is 96.8～97.5 ℃, water extraction 15 in the cat head phase splitter, oil phase refluxes, and the discharging of tower still is a n-propyl alcohol 16; Separating Tata still aqueous acetic acid 13, to enter theoretical plate number be 10 acetic acid extraction tower 4, and extraction agent is selected TERTIARY BUTYL AMINE for use, and extraction agent and raw material ratio are 5, and service temperature is 35 ℃, and acetic acid extraction tower cat head obtains acetic acid, extractant mixture 17, and the tower still is a waste water 18; Acetic acid, extractant mixture enter extraction agent recovery tower 5, theoretical plate number is 10, feed entrance point is the 4th a block of theoretical tray, reflux ratio is 6, the control tower top temperature is 115～118 ℃, and overhead distillate is an acetic acid 19, and the tower still obtains reclaiming extraction agent 20, behind the stable operation, the logistics analysis data of each tower see Table 1.
The logistics analysis data (weight %) of each tower of table 1
[embodiment 2]
By flow process shown in Figure 1, (boiling point is less than 40 ℃ component for aqueous phase byproduct from Fischer-Tropsch synthesis 6, boiling range be 50～120 ℃ component and boiling point greater than 120 ℃ component account for respectively that weight forms 5%, 85% and 10%) entering number of theoretical plate is 60 common rectifying tower 1, feed entrance point is the 35th a block of theoretical tray, reflux ratio is 1, the control tower top temperature is 40 ℃, it from the 40th theoretical tray side line extraction boiling range 50～120 ℃ cut 8, it is 200 separation tower 2 that side stream 8 enters number of theoretical plate, the number of theoretical plate on division plate top is 40, the bottom number of theoretical plate also is 60, the liquid phase distribution mark of division plate upper left-hand is 0.31, the gas phase distribution mark of lower left side is 0.3, reflux ratio is 30, tower top temperature is controlled to be 60～64 ℃, last side line extraction temperature is controlled to be 68～68.5 ℃, following side line extraction temperature is controlled to be 87～93 ℃, overhead fraction acetone and carbinol mixture 10, separating tower top side line extraction is ethanol 11, separating the tower bottom side line extraction n-propyl alcohol aqueous solution 12, to enter theoretical plate number be 60 azeotropy rectification column 3, feed entrance point is the 35th a block of theoretical tray, entrainer is selected n-butyl acetate for use, entrainer and raw material ratio are 0.2, control tower still temperature is 96.8～97.5 ℃, water extraction 15 in the cat head phase splitter, oil phase refluxes, and the discharging of tower still is a n-propyl alcohol 16; Separating Tata still aqueous acetic acid 13, to enter theoretical plate number be 40 acetic acid extraction tower 4, and extraction agent is selected TERTIARY BUTYL AMINE for use, and extraction agent and raw material ratio are 1, and service temperature is 35 ℃, and acetic acid extraction tower cat head obtains acetic acid, extractant mixture 17, and the tower still is a waste water 18; Acetic acid, extractant mixture enter extraction agent recovery tower 5, theoretical plate number is 50, feed entrance point is the 20th a block of theoretical tray, reflux ratio is 1, the control tower top temperature is 115～118 ℃, and overhead distillate is an acetic acid 19, and the tower still obtains reclaiming extraction agent 20, behind the stable operation, the logistics analysis data of each tower see Table 1.
The logistics analysis data (weight %) of each tower of table 2
[embodiment 3]
By flow process shown in Figure 1, (boiling point is less than 40 ℃ component for aqueous phase byproduct from Fischer-Tropsch synthesis 6, boiling range be 50～120 ℃ component and boiling point greater than 120 ℃ component account for respectively that weight forms 5%, 85% and 10%) entering number of theoretical plate is 30 common rectifying tower 1, feed entrance point is the 17th a block of theoretical tray, reflux ratio is 3, the control tower top temperature is 40 ℃, it from the 20th theoretical tray side line extraction boiling range 50～120 ℃ cut 8, it is 120 separation tower 2 that side stream 8 enters number of theoretical plate, the number of theoretical plate on division plate top is 20, the bottom number of theoretical plate also is 30, the liquid phase distribution mark of division plate upper left-hand is 0.52, the gas phase distribution mark of lower left side is 0.5, reflux ratio is 12, tower top temperature is controlled to be 60～64 ℃, last side line extraction temperature is controlled to be 68～68.5 ℃, following side line extraction temperature is controlled to be 87～93 ℃, overhead fraction acetone and carbinol mixture 10, separating tower top side line extraction is ethanol, separating the tower bottom side line extraction n-propyl alcohol aqueous solution, to enter theoretical plate number be 30 azeotropy rectification column 3, feed entrance point is the 17th a block of theoretical tray, entrainer is selected Iso Butyl Acetate for use, entrainer and raw material ratio are 0.5, control tower still temperature is 96.8～97.5 ℃, water extraction 15 in the cat head phase splitter, oil phase refluxes, and the discharging of tower still is a n-propyl alcohol 16; Separating Tata still aqueous acetic acid 13, to enter theoretical plate number be 20 acetic acid extraction tower 4, extraction agent is selected trialkyl phosphine for use, and extraction agent and raw material ratio are 2, and service temperature is 35 ℃, acetic acid extraction tower cat head obtains acetic acid, extractant mixture 17, and the tower still is a waste water 18; Acetic acid, extractant mixture enter extraction agent recovery tower 5, theoretical plate number is 25, feed entrance point is the 10th a block of theoretical tray, reflux ratio is 3, the control tower top temperature is 115～118 ℃, and overhead distillate is an acetic acid 19, and the tower still obtains reclaiming extraction agent 20, behind the stable operation, the logistics analysis data of each tower see Table 1.
The logistics analysis data (weight %) of each tower of table 3
[embodiment 4]
Change the composition of aqueous phase byproduct from Fischer-Tropsch synthesis, boiling point less than 40 ℃ component, component that boiling range is 50～120 ℃ and boiling point greater than 120 ℃ component account for respectively that weight forms 7%, 84% and 9%, keep other each conditions such as embodiment 3, behind the stable operation, the logistics analysis data of each tower see Table 4.
The logistics analysis data (weight %) of each tower of table 4
Claims (5)
1, a kind of method of separating aqueous phase byproduct from Fischer-Tropsch synthesis may further comprise the steps:
A, aqueous phase by-product enter the middle part of common rectifying tower (1), and side line extraction boiling range is 50～120 ℃ a cut stream I, and cat head obtains boiling point less than 40 ℃ light constituent, and the tower still obtains boiling point greater than 120 ℃ heavy constituent;
B, stream I enter the middle part of separating tower (2) left side, and overhead distillate is methyl alcohol and acetone soln, and the tower still obtains aqueous acetic acid stream I I, side line extraction ethanol on the right side, following side line extraction n-propyl alcohol aqueous solution stream I II;
C, stream I II enter the middle part of azeotropy rectification column (3), water extraction in the cat head phase splitter, and oil phase refluxes, and the discharging of tower still is a n-propyl alcohol, and wherein entrainer is selected from water and forms at least a in the minimum azeotropic mixture;
D, stream I I enter the cat head of acetic acid extraction tower (4), and acetic acid extraction tower cat head obtains acetic acid, extractant mixture stream I V, and the tower still is a waste water, and wherein extraction agent is selected from least a in organic phosphine or the organic amine;
E, stream I V enter the middle part of extraction agent recovery tower (5), and overhead distillate is an acetic acid, and the tower still obtains reclaiming extraction agent.
2, according to the method for right 1 described separation aqueous phase byproduct from Fischer-Tropsch synthesis, it is characterized in that the common rectifying tower theoretical plate number is 10～60, reflux ratio is 1～12, tower top temperature control is not less than 40 ℃; The azeotropy rectification column theoretical plate number is 15～60, and entrainer and raw material ratio are 0.2～1, and control tower still temperature is 96.8～97.5 ℃; Acetic acid extraction tower theoretical plate number is 10～40, and extraction agent and raw material ratio are 1～6, normal-temperature operation; Extraction agent recovery tower theoretical plate number is 10～50, and reflux ratio is 1～6, decompression operation.
3, according to the method for right 1 described separation aqueous phase byproduct from Fischer-Tropsch synthesis, it is characterized in that separating the tower theoretical plate number is 50～200, division plate top accounts for 1/6～1/3 theoretical stage, the division plate bottom accounts for 1/6～1/3 theoretical stage, the left side liquid phase distribution mark on division plate top is 0.3～0.7, the left side gas phase distribution mark of division plate bottom is 0.3～0.7, reflux ratio is 5～30, tower top temperature is controlled to be 60～64 ℃, last side line extraction temperature is controlled to be 68～68.5 ℃, and following side line extraction temperature is controlled to be 87～93 ℃.
4,, it is characterized in that the used entrainer of azeotropy rectification column is at least a in hexanaphthene, Iso Butyl Acetate or the n-butyl acetate according to the separation method of right 1 described aqueous phase by-product of fischer-tropsch synthesis reaction.
5,, it is characterized in that the selected extraction agent of extraction tower is at least a in trialkyl phosphine or the TERTIARY BUTYL AMINE according to the separation method of right 1 described aqueous phase by-product of fischer-tropsch synthesis reaction.
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| CN2008100432527A CN101555193B (en) | 2008-04-11 | 2008-04-11 | Separating method of aqueous phase byproduct from Fischer-Tropsch synthesis |
| RU2009102120/04A RU2480445C2 (en) | 2008-01-23 | 2009-01-22 | Method of separating liquid phase by-products of fischer-tropsch synthesis |
| ZA2009/00548A ZA200900548B (en) | 2008-01-23 | 2009-01-23 | Process for separating by-products in aqueous phase of a fischer-tropsch synthesis |
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Cited By (6)
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| CN102060660A (en) * | 2010-12-13 | 2011-05-18 | 上海兖矿能源科技研发有限公司 | Method for separating alcohol compound from Tropsch synthesis reaction water |
| CN104150670A (en) * | 2014-08-29 | 2014-11-19 | 神华集团有限责任公司 | Processing device and method for Fischer-Tropsch synthetic water |
| CN105669377A (en) * | 2016-01-22 | 2016-06-15 | 北京凯文特科技有限公司 | Technique for separating mixed alcohol |
| CN109796310A (en) * | 2019-03-26 | 2019-05-24 | 河北工业大学 | A method of initial gross separation being carried out to F- T synthesis water using next door rectifying column |
| CN109824480A (en) * | 2019-02-27 | 2019-05-31 | 北控城市(北京)环境科技有限公司 | The process of ethyl alcohol in a kind of separating-purifying coal oil rectification residue |
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| CN1297523C (en) * | 2005-04-01 | 2007-01-31 | 上海兖矿能源科技研发有限公司 | Method for treating water reacted from Fischer-Tropsch synthesis |
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| CN102060660A (en) * | 2010-12-13 | 2011-05-18 | 上海兖矿能源科技研发有限公司 | Method for separating alcohol compound from Tropsch synthesis reaction water |
| CN102060660B (en) * | 2010-12-13 | 2013-07-03 | 上海兖矿能源科技研发有限公司 | Method for separating alcohol compound from Tropsch synthesis reaction water |
| CN104150670A (en) * | 2014-08-29 | 2014-11-19 | 神华集团有限责任公司 | Processing device and method for Fischer-Tropsch synthetic water |
| CN104150670B (en) * | 2014-08-29 | 2015-10-14 | 神华集团有限责任公司 | The treatment unit of F-T synthesis water and treatment process |
| CN105669377A (en) * | 2016-01-22 | 2016-06-15 | 北京凯文特科技有限公司 | Technique for separating mixed alcohol |
| CN105669377B (en) * | 2016-01-22 | 2019-01-29 | 北京凯文特科技有限公司 | A kind of process separating mixed alcohol |
| CN109824480A (en) * | 2019-02-27 | 2019-05-31 | 北控城市(北京)环境科技有限公司 | The process of ethyl alcohol in a kind of separating-purifying coal oil rectification residue |
| CN109824480B (en) * | 2019-02-27 | 2023-01-20 | 北京精刻环保科技有限公司 | Process method for separating and purifying ethanol in coal-to-liquids rectification residues |
| CN109796310A (en) * | 2019-03-26 | 2019-05-24 | 河北工业大学 | A method of initial gross separation being carried out to F- T synthesis water using next door rectifying column |
| CN111518593A (en) * | 2020-04-23 | 2020-08-11 | 河北工业大学 | Method for primarily separating byproduct mixed alcohol in coal indirect liquefaction process |
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