CN117023703A - Fischer-Tropsch synthesis water oil removal method - Google Patents
Fischer-Tropsch synthesis water oil removal method Download PDFInfo
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- CN117023703A CN117023703A CN202310733298.6A CN202310733298A CN117023703A CN 117023703 A CN117023703 A CN 117023703A CN 202310733298 A CN202310733298 A CN 202310733298A CN 117023703 A CN117023703 A CN 117023703A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 280
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 99
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 54
- 239000012071 phase Substances 0.000 claims abstract description 139
- 238000000926 separation method Methods 0.000 claims abstract description 45
- 239000008346 aqueous phase Substances 0.000 claims abstract description 37
- 239000000126 substance Substances 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 239000003921 oil Substances 0.000 claims description 119
- 239000012530 fluid Substances 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 27
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 24
- 229910052760 oxygen Inorganic materials 0.000 claims description 24
- 239000001301 oxygen Substances 0.000 claims description 24
- 230000003068 static effect Effects 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 15
- 238000000746 purification Methods 0.000 claims description 15
- 239000000295 fuel oil Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 4
- 238000011143 downstream manufacturing Methods 0.000 claims description 2
- 238000005485 electric heating Methods 0.000 claims description 2
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- 239000000047 product Substances 0.000 description 129
- 235000019198 oils Nutrition 0.000 description 103
- 238000004821 distillation Methods 0.000 description 22
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- 229930195733 hydrocarbon Natural products 0.000 description 12
- 150000002430 hydrocarbons Chemical class 0.000 description 12
- 238000009826 distribution Methods 0.000 description 11
- 239000004215 Carbon black (E152) Substances 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 150000007513 acids Chemical class 0.000 description 6
- 150000001298 alcohols Chemical class 0.000 description 6
- 238000005238 degreasing Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 4
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 4
- 150000001299 aldehydes Chemical class 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 150000002576 ketones Chemical class 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000001223 reverse osmosis Methods 0.000 description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 2
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- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 235000019476 oil-water mixture Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
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- 239000000243 solution Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/365—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds from petrochemical industry (e.g. refineries)
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/04—Flow arrangements
- C02F2301/043—Treatment of partial or bypass streams
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/14—Maintenance of water treatment installations
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention provides a method for removing oil from Fischer-Tropsch synthesis water, which comprises the following steps: the emulsified Fischer-Tropsch synthesis water is fed into a raw material water tank for standing, an oil phase product and an aqueous phase product are obtained through separation, and oil-water separation is carried out after the aqueous phase product and oily substances are mixed at a high temperature, so that the purpose of removing oil from the Fischer-Tropsch synthesis water is realized. The method can be advantageously used for removing oil from emulsified Fischer-Tropsch synthesis water, and the emulsified oil contained in the Fischer-Tropsch synthesis water is obtained through effective separation, so that the oil content in the obtained Fischer-Tropsch synthesis water is greatly reduced, the COD in the wastewater is greatly reduced, the oil yield is effectively improved, and the economic benefit is improved.
Description
Technical Field
The invention belongs to the field of chemical wastewater purification treatment, and particularly relates to a Fischer-Tropsch synthesis water deoiling method.
Background
The Fischer-Tropsch synthesis reaction is to convert carbon-containing materials such as coal, natural gas, biomass, organic garbage, sludge and the like into synthesis gas (CO and H) 2 ) Then the catalyst is converted into hydrocarbon organic matters (mainly comprising normal paraffins, a small amount of isoparaffins, olefins and the like) through a specific catalyst, and a large amount of water and part of low-carbon-number oxygen-containing organic matters (mainly alcohols, aldehydes, ketones, acids, esters and the like) are also generated, and a large amount of heat is discharged. In the iron-based Fischer-Tropsch synthesis reaction process, the yield of water is generally more than one time that of a synthetic oil product.
After the Fischer-Tropsch synthesis reaction, the generated Fischer-Tropsch synthesis water and Fischer-Tropsch synthesis hydrocarbons need to be separated, and the preliminary separation process can be described as: the gas phase product of the Fischer-Tropsch reactor is subjected to cooling flash evaporation, a part of the gas phase product is cooled into liquid phase fluid, and the liquid phase fluid is separated into aqueous phase fluid containing a small amount of dissolved organic matters (hydrocarbon and oxygen-containing organic matters) and trace suspended matters through an oil-water separator, namely Fischer-Tropsch synthesis water to be treated in the invention.
In the Fischer-Tropsch synthesis process, the composition of the produced Fischer-Tropsch synthesis aqueous phase byproducts is different due to the different Fischer-Tropsch synthesis process technology, fischer-Tropsch synthesis catalyst and synthesis reaction operation parameters. Generally, the Fischer-Tropsch synthesis water phase has a water content of 70wt% to 97wt% and an organic oxygenate content of 3wt% to 30wt%. The applicant adopts the high-temperature slurry bed iron-based Fischer-Tropsch synthesis technology of the middle-branch of synthetic oil technology Co., ltd, according to the data of Fischer-Tropsch synthesis water provided by the current commercialized project, the composition of the Fischer-Tropsch synthesis water is water, the content of various hydrocarbons of C5-C20 is generally lower than 1000ppm, the carbon number of oxygen-containing organic matters is generally lower than 8, the content of alcohols (C1-C8 alcohols) is generally not higher than 2wt%, the content of acids (C1-C6 acids) is generally not higher than 1wt%, and the content sum of aldehydes (acetaldehyde and propionaldehyde), ketones (acetone and butanone), esters (ethyl formate and ethyl acetate) is not higher than 0.5 wt%; cod=15000 to 60000mg/L; ph=2 to 4; the total oil is not higher than 2000mg/L, and the petroleum is not higher than 1000mg/L.
Because of the existence of hydrocarbon and oxygen-containing organic matters, fischer-Tropsch synthesis water does not meet the standard of emission or recycling, and especially acid organic matters in the Fischer-Tropsch synthesis water can also cause corrosion to equipment. And therefore require disposal prior to discharge or use. This is necessary to reduce environmental pollution, recover high added value organics, and increase the economic benefit of the fischer-tropsch process.
Several patent technologies have been reported for recycling Fischer-Tropsch synthesis water, such as ZL03814122.1, ZL03814125.6 and ZL03814127.2, each of which discloses a method for purifying Fischer-Tropsch reaction water. The main process operating units involved in the patent include: common rectification, evaporation, extraction, biological treatment, solid-liquid separation, reverse osmosis and the like. In the related flow, the water-containing substance at the bottom of the rectifying tower is firstly biologically treated and then subjected to reverse osmosis to obtain high-purity water. In addition, ZL201010512405.5, ZL201310368576.9, ZL201310424500.3 and ZL 2015194055. X each disclose a method for separating and recovering an organic oxygen-containing compound in a fischer-tropsch synthesis aqueous phase, and the main operation units involved in the patent include: acid-base neutralization, rectification, reverse osmosis, biological treatment, advanced oxidation, and the like. And adding inorganic alkali into Fischer-Tropsch synthesis water to neutralize carboxylic acid in the Fischer-Tropsch synthesis water to generate carboxylate, regulating the pH value to be neutral, and then sending the neutralized Fischer-Tropsch synthesis water into a rectifying tower for rectifying, so that corrosion to equipment is reduced.
In the above patent technology, whether the organic matters in the Fischer-Tropsch synthesis water are recycled or the Fischer-Tropsch synthesis water is purified, the Fischer-Tropsch synthesis water needs to be subjected to oil removal operation first, which is also a key for determining whether the above patent technology can be successfully implemented. However, in the whole commercial project operation process, after the gas phase product of the Fischer-Tropsch reactor is cooled by cooling flash evaporation, the obtained fluid enters an oil-water separator and can not completely separate oil from water, meanwhile, because the gas phase product at the top of the reactor also contains small-size catalyst particles, when a coalescer is further adopted for oil removal, the large-area blockage of the coalescer is caused, so that the whole oil removal unit does not normally operate, the treatment load is greatly reduced, the water quality index at the outlet of the oil removal unit can not meet the design requirement, the stable operation of a downstream synthetic water treatment unit can be influenced when serious, the stagnation of the synthetic water treatment process is finally caused until the oil removal process is stopped, and therefore, the stable operation of the oil removal process also relates to the stable operation of the whole production process, which is very important for the Fischer-Tropsch commercial project.
In addition, in the oil-water separation process of Fischer-Tropsch synthesis water, the problem of oil-water emulsification often exists, so that the oil content in the water phase product after primary separation is still high, and if the emulsification state of Fischer-Tropsch synthesis water cannot be fundamentally solved, adverse effects still exist on the purification and separation process of Fischer-Tropsch synthesis water.
Disclosure of Invention
In view of the above problems, the present invention provides a method for removing oil from fischer-tropsch synthesis water, which has a simple process and can be operated continuously in industry, by transferring the emulsified oil in the aqueous phase product separated from the fischer-tropsch synthesis water to the oil phase at a high temperature in an oil-water mixing manner and separating the oil from the water phase product through an oil-water separator, thereby demulsifying the aqueous phase product and removing the emulsified oil in the aqueous phase product from the aqueous phase product.
In one aspect, the invention provides a method for removing oil from Fischer-Tropsch synthesis water, comprising:
(1) Feeding the emulsified Fischer-Tropsch synthesis water into a raw material water tank for standing, and separating to obtain an oil phase product and a water phase product;
(2) Heating the water phase product to not lower than 80 ℃ by a heat exchanger, and then mixing the water phase product with oily substances to obtain mixed liquid, wherein the oily substances are Fischer-Tropsch synthesis light oil, fischer-Tropsch synthesis heavy oil and/or Fischer-Tropsch synthesis heavy wax, and the volume ratio of the water phase product to the oily substances is 1:10-10:1;
(3) Feeding the mixed solution into an oil-water separator for oil-water separation;
(4) Mixing part or all of the oil phase product from the oil-water separator with the oil phase product from the raw material water tank and outputting the mixture to a downstream unit;
(5) And carrying out heat exchange and cooling on the water phase fluid obtained by separation in the oil-water separator, and then sending the water phase fluid into a synthetic water treatment unit after filtering to carry out separation of oxygen-containing organic matters and purification treatment of synthetic water.
The removal of oil from emulsified Fischer-Tropsch water by the method of the invention may present the following technical advantages, but is not limited thereto:
1. the method is continuous operation, the treatment capacity can be adjusted according to the actual requirements of the factory site, the industrial implementation is easy, the investment and the operation cost are low, and the method is environment-friendly;
2. the oily substances used in the invention are Fischer-Tropsch synthesis products, can be recycled, effectively reduce the process cost, and do not introduce impurities outside the system;
3. the method can be advantageously used for removing oil from emulsified Fischer-Tropsch synthesis water, and can be used for effectively separating to obtain emulsified oil contained in the Fischer-Tropsch synthesis water, and delivering the emulsified oil to a downstream unit for treatment, so that the oil yield is effectively improved, and the economic benefit is improved;
4. the oil content in the Fischer-Tropsch synthesis water obtained after the oil removal by adopting the method provided by the invention is greatly reduced, the COD in the wastewater is greatly reduced, and the method has good environmental benefits.
Drawings
FIG. 1 is a schematic flow diagram of an exemplary Fischer-Tropsch synthesis water degreasing process of the invention.
Wherein each reference numeral is as follows: t1 raw material water tank; a P1 feed pump; m1 static mixer; a T2 oil-water separator; e1 heat exchanger;
101 Fischer-Tropsch synthesis water, 102 an oil phase product of a raw material water tank, 103 an aqueous phase product of the raw material water tank, 104, 105 mixed liquor, 106 an oil phase product discharged from an oil-water separator, 107 a part of the oil phase product 106, and 108 another part of the oil phase product 106; 109 aqueous phase fluid.
Detailed Description
The following describes exemplary embodiments of the present invention, but those skilled in the art will understand that the scope of the present invention is not limited thereto.
In this context, unless otherwise indicated, the term "part" or "portion" means that the object it modifies is present in an amount of more than 0% to less than 100% relative to the total amount of the like.
Herein, unless otherwise indicated, the term "room temperature" refers to a temperature of 10 ℃ to 40 ℃.
In one embodiment, the invention relates to a method for removing oil from Fischer-Tropsch synthesis water, comprising:
(1) Feeding the emulsified Fischer-Tropsch synthesis water into a raw material water tank for standing, and separating to obtain an oil phase product and a water phase product;
(2) Heating the water phase product to not lower than 80 ℃ by a heat exchanger, and then mixing the water phase product with oily substances to obtain mixed liquid, wherein the oily substances are Fischer-Tropsch synthesis light oil, fischer-Tropsch synthesis heavy oil and/or Fischer-Tropsch synthesis heavy wax, and the volume ratio of the water phase product to the oily substances is 1:10-10:1;
(3) Feeding the mixed solution into an oil-water separator for oil-water separation;
(4) Mixing part or all of the oil phase product from the oil-water separator with the oil phase product from the raw material water tank and outputting the mixture to a downstream unit;
(5) And carrying out heat exchange and cooling on the water phase fluid obtained by separation in the oil-water separator, and then sending the water phase fluid into a synthetic water treatment unit after filtering to carry out separation of oxygen-containing organic matters and purification treatment of synthetic water.
The Fischer-Tropsch synthesis water is an aqueous phase fluid containing a small amount of dissolved organic matters (hydrocarbon and oxygen-containing organic matters) and a trace amount of suspended matters, which is obtained by cooling and flashing a gas phase product of a Fischer-Tropsch synthesis reactor, cooling a part of the gas phase product into a liquid phase fluid, and separating the liquid phase fluid through a separator.
In some embodiments, in step (1), the total content of oxygenates in the fischer-tropsch synthesis water may be from 2wt% to 5wt%; cod=15000 to 60000mg/L (e.g. 15000 to 55000 mg/L); ph=2 to 4 (e.g., 2.5 to 3.5); the total oil is not higher than 10000mg/L (for example, 500mg/L to 2000 mg/L), and the petroleum is not higher than 2000mg/L (for example, 100mg/L to 1000 mg/L). Wherein the oxygenate comprises alcohols, aldehydes, acids, esters and ketones, and the like, wherein the alcohols (predominantly C1-C8 alcohols) are typically present in an amount of no greater than 3wt%, the acids (predominantly C1-C6 acids) are typically present in an amount of no greater than 2wt%, and the aldehydes (predominantly acetaldehyde and propionaldehyde), ketones (predominantly acetone and butanone) and esters (predominantly ethyl formate, ethyl acetate) are present in an amount of no greater than 1wt%, relative to the total weight of the Fischer-Tropsch synthesis water.
In some embodiments, in step (2), the aqueous phase product is heated to 80 ℃ to 300 ℃, e.g., 150 ℃ to 240 ℃ via a heat exchanger. In order to prevent gasification of the water in the aqueous product after the temperature of the aqueous product increases, it is necessary to apply a very high pressure to the degreasing system (i.e., the system for carrying out step (2)) when the temperature is too high (therefore, it is preferable to heat the aqueous product to 300 ℃ or less, more preferably 240 ℃ or less via a heat exchanger to ensure smooth and long-term operation of the reaction system and to reduce the adverse effect of the excessively high pressure required for maintaining the excessively high temperature on the system), for example, a back pressure may be applied to the degreasing system by introducing into the systemN 2 Or water vapor, or may be implemented by water gasification self-pressurization within the system. The back pressure should be no lower than the saturated vapor pressure of vapor at the temperature of the water phase product in the oil removal system after heat exchange. In this context, the degreasing system back pressure (i.e. the pressure of step (2)) is 1 atm or higher, for example, the degreasing system back pressure should be not lower than 0.5MPa when the aqueous phase product is heated to 150 ℃, and the degreasing system back pressure should be not lower than 4.0MPa when the aqueous phase product is heated to 250 ℃, so that the mixing is performed at the back pressure.
In some embodiments, in step (2), the volume ratio of the aqueous phase product to the oily substance may be from 1:5 to 5:1, more preferably may be from 1:2 to 2:1, for example from 1:1 to 2:1.
In some embodiments, in step (2), the aqueous phase product is mixed with oily substances using a static mixer. The mixing can be used for extracting the emulsified oil product and the oxygen-containing organic matters carried in the water phase product into the oil phase, so that the water phase product can be demulsified, and the emulsified oil can be separated out.
In some embodiments, in step (2), the Fischer-Tropsch synthesis light oil may be hydrocarbons and oxygenated organics having a carbon number distribution of approximately C4-C37 at a distillation range temperature of 0 ℃ to 500 ℃, IBP=0 ℃ to 50 ℃, FBP=300 ℃ to 500 ℃,50% distillation temperature 150 ℃ to 250 ℃; the Fischer-Tropsch synthesis heavy oil can be hydrocarbon with carbon number distribution similar to C6-C54 and oxygen-containing organic matters, wherein the distillation range temperature is 100-700 ℃, IBP=100-200 ℃, FBP=500-700 ℃,50% distillation temperature is 300-400 ℃; the Fischer-Tropsch synthesis heavy wax can be hydrocarbon and oxygen-containing organic matters with carbon number distribution of C8-C90 and above, wherein the distillation range temperature is 200-750 ℃, IBP=200-300 ℃, FBP=650-750 ℃, and 50% distillation temperature is 500-600 ℃.
In some embodiments, in step (3), the temperature at which the oil-water separator is operated may be the same or substantially the same as the temperature of the aqueous phase product after heating by the heat exchanger, for example may be 80 ℃ to 300 ℃, preferably 80 ℃ to 240 ℃; the pressure is 0 to 5MPa, preferably 0.1 to 3.5MPa, for example 0.1 to 2.5MPa, in terms of gauge pressure.
In some embodiments, in step (4), a portion of the oil phase product exiting the oil-water separator may be returned to step (2) for remixing with the aqueous phase product (e.g., by returning to the static mixer inlet), thereby allowing recycling of the oil phase product from the oil-water separator; at this time, the other part of the oil phase product from the oil-water separator can be mixed with the oil phase product from the raw material water tank and then output to a downstream unit for further treatment.
In some embodiments, the volume ratio between the oil phase product exiting the oil-water separator returned to step (2) and the oil phase product exiting the oil-water separator output to the downstream unit is from 10:1 to 1:10, such as from 10:1 to 1:1 (e.g., 5:1, 2:1).
In some further preferred embodiments, in step (5), the heat exchange cooling may comprise cooling to room temperature, or may also be cooling to a downstream unit treatment temperature as required by a downstream treatment unit (e.g., a synthetic water treatment unit). As an example, in step (5), the aqueous phase fluid may be subjected to heat exchange to a temperature of 20 ℃ to 60 ℃, for example 30 ℃ to 50 ℃.
In some further preferred embodiments, in step (5) suspended particles in the aqueous phase fluid are removed by said filtration, preferably by a filter cartridge having a pore size of not more than 10 μm, preferably not more than 5 μm, more preferably not more than 1 μm. And then, sending the filtered water phase fluid into a synthetic water treatment unit for separation of oxygen-containing organic matters and purification treatment of synthetic water, so as to further improve the quality of water products.
In some preferred embodiments, the present invention also provides a method for removing oil from Fischer-Tropsch synthesis water, comprising the steps of:
(i) Feeding the emulsified Fischer-Tropsch synthesis water 101 into a raw material water tank T1 for standing, and separating to obtain an oil phase product 102 and a water phase product 103;
(ii) After being fed into a heat exchanger E1 through a feed pump P1 and heated to not lower than 80 ℃, the water phase product 103 is mixed with oily substances 104 in a static mixer M1 to obtain a mixed solution 105, wherein the oily substances are Fischer-Tropsch synthesis light oil, fischer-Tropsch synthesis heavy oil and/or Fischer-Tropsch synthesis heavy wax, and the volume ratio of the water phase product to the oily substances is 1:10 to 10:1;
(iii) Feeding the mixed solution 105 into an oil-water separator T2 for oil-water separation;
(iv) Mixing a part 107 of the oil phase product 106 from the oil-water separator T2 with the oil phase product 102 from the raw material water tank, outputting the mixture to a downstream unit, and returning the other part 108 of the oil phase product 106 to the inlet of the static mixer M1 to be mixed with the water phase product 103 again;
(v) And carrying out heat exchange and cooling on the water phase fluid 109 obtained by separation in the oil-water separator T2, and directly sending the water phase fluid into a synthetic water treatment unit after filtering to carry out separation of oxygen-containing organic matters and purification treatment of synthetic water.
In some embodiments, the raw material water tank T1, the static mixer M1, and the oil-water separator T2 may be normal pressure and/or high pressure equipment according to mixing conditions, and the temperature and pressure resistant conditions may be determined according to material properties and mixing and separation conditions.
In some embodiments, the heat exchanger may be a sleeve heat exchanger, a plate heat exchanger, etc., and the heat exchange mode of the heat exchanger may be steam or electric heating. When steam is used for heat exchange, the heat exchanged steam can be saturated steam of 0.5MPa, 1.5MPa, 2.0MPa, 2.5MPa, 3.0MPa, 4.0MPa, 5.0MPa or 6.0MPa,
in some embodiments, the volume ratio of the oil-water mixture may be 1:5 to 5:1, more preferably may be 1:2 to 2:1, for example 1:1 to 2:1.
In some embodiments, the Fischer-Tropsch synthesis light oil can be hydrocarbons with a carbon number distribution of approximately C4-C37 and oxygen-containing organics with a distillation range temperature of 0 ℃ to 500 ℃, IBP=0 ℃ to 40 ℃, FBP=300 ℃ to 500 ℃,50% distillation temperature of 150 ℃ to 250 ℃; the Fischer-Tropsch synthesis heavy oil can be hydrocarbon with carbon number distribution similar to C6-C54 and oxygen-containing organic matters, wherein the distillation range temperature is 100-700 ℃, IBP=100-200 ℃, FBP=500-700 ℃,50% distillation temperature is 300-400 ℃; the Fischer-Tropsch synthesis heavy wax can be hydrocarbon and oxygen-containing organic matters with carbon number distribution of C8-C90 and above, wherein the distillation range temperature is 200-750 ℃, IBP=200-300 ℃, FBP=650-750 ℃, and 50% distillation temperature is 500-600 ℃. The oil-water separator T4 performs oil-water separation according to the density difference of the Fischer-Tropsch synthesis product and water, and in order to improve the separation efficiency, separation internals such as baffle plates, coalescing plates and the like can be added in the oil-water separator, for example, turbulent flow after oil and water are mixed can be formed into laminar flow through the baffle plates, and the oil-water separation efficiency is further improved through the coalescing action of the coalescing plates.
Taking Fischer-Tropsch synthesis heavy wax as an example, the operating temperature of the oil-water separator T2 can be 150-240 ℃, preferably 180-230 ℃; the pressure is 0 to 5MPa, preferably 0.1 to 3.5MPa, for example 0.1 to 2.5MPa, in terms of gauge pressure.
In some embodiments, a portion 107 of the oil phase product 106 is output to a downstream unit and another portion 108 (or mixed with externally introduced material as stream 104) is returned to the inlet of static mixer M1 for secondary mixing with the aqueous phase product 103, wherein the volume ratio between the returned 108 and the output 107 to the downstream unit is 10:1 to 1:10, preferably 10:1 to 1:1.
In some embodiments, the filtration is performed to remove suspended particles from the aqueous fluid, for example, by using a filter element having a pore size of not more than 10 μm, preferably not more than 5 μm, and more preferably not more than 1 μm, and the aqueous fluid is fed to a synthetic water treatment unit after filtration for separation of oxygenates and purification of synthetic water.
Hereinafter, the solution of the present invention is further explained by what is shown in the following numbered paragraphs:
1. a method for removing oil from fischer-tropsch synthesis water, comprising:
(1) Feeding the emulsified Fischer-Tropsch synthesis water into a raw material water tank for standing, and separating to obtain an oil phase product and a water phase product;
(2) Heating the water phase product to not lower than 80 ℃ by a heat exchanger, and then mixing the water phase product with oily substances to obtain mixed liquid, wherein the oily substances are Fischer-Tropsch synthesis light oil, fischer-Tropsch synthesis heavy oil and/or Fischer-Tropsch synthesis heavy wax, and the volume ratio of the water phase product to the oily substances is 1:10-10:1;
(3) Feeding the mixed solution into an oil-water separator for oil-water separation;
(4) Mixing part or all of the oil phase product from the oil-water separator with the oil phase product from the raw material water tank and outputting the mixture to a downstream unit;
(5) And carrying out heat exchange and cooling on the water phase fluid obtained by separation in the oil-water separator, and then sending the water phase fluid into a synthetic water treatment unit after filtering to carry out separation of oxygen-containing organic matters and purification treatment of synthetic water.
2. The method of paragraph 1 wherein in step (1) the total oxygenate content in the Fischer-Tropsch synthesis water is from 2wt% to 5wt%; cod=15000 to 60000mg/L; ph=2 to 4; the total oil is not higher than 10000mg/L, and petroleum is not higher than 2000mg/L.
3. The process of paragraph 1 or 2 wherein, in step (2), the aqueous phase product is heated to 80 ℃ to 300 ℃ via a heat exchanger.
4. The method of any of paragraphs 1-3, wherein, in step (2), the mixing is performed at 1 normal atmospheric pressure or higher.
5. The method of any of paragraphs 1-4, wherein in step (2), the volume ratio of the aqueous phase product to the oily substance is from 1:5 to 5:1.
6. The method of any of paragraphs 1-5, wherein in step (2), the aqueous phase product is mixed with the oily substance using a static mixer.
7. The method of any one of paragraphs 1-6, wherein, in step (3), the oil-water separator is operated at a temperature of 80℃to 300 ℃; the pressure is 0-5 MPa based on gauge pressure.
8. The method of any one of paragraphs 1-7, wherein in step (4), a portion of the oil phase product exiting the oil-water separator may be returned to step (2) for re-mixing with the aqueous phase product, and another portion of the oil phase product exiting the oil-water separator is mixed with the oil phase product exiting the feed water tank for further processing, and output to a downstream unit.
9. The method of paragraph 8, wherein the volume ratio between the oil phase product exiting the oil-water separator returned to step (2) and the oil phase product exiting the oil-water separator output to a downstream unit is from 10:1 to 1:10.
10. The method of any of paragraphs 1-9, wherein in step (5), the heat exchange cooling comprises cooling to room temperature or cooling to a downstream unit process temperature as required by the downstream process unit.
11. The method of any one of paragraphs 1-10, wherein in step (5), the aqueous fluid is heat exchanged to a temperature of 20-60 ℃.
12. The method of any one of paragraphs 1-11, wherein in step (5), the filtering is performed with a filter cartridge having a pore size of no greater than 10 μm.
13. The method of any one of paragraphs 1-12, comprising the steps of:
(i) Feeding the emulsified Fischer-Tropsch synthesis water into a raw material water tank for standing, and separating to obtain an oil phase product and a water phase product;
(ii) The water phase product is fed into a heat exchanger through a feed pump to be heated to not lower than 80 ℃, and then is mixed with oily substances in a static mixer to obtain mixed liquid, wherein the oily substances are Fischer-Tropsch synthesis light oil, fischer-Tropsch synthesis heavy oil and/or Fischer-Tropsch synthesis heavy wax, and the volume ratio of the water phase product to the oily substances is 1:10-10:1;
(iii) Feeding the mixed solution into an oil-water separator for oil-water separation;
(iv) Mixing one part of the oil phase product from the oil-water separator with the oil phase product from the raw material water tank, outputting the mixture to a downstream unit, and returning the other part of the oil phase product from the oil-water separator to an inlet of a static mixer to be mixed with the water phase product again;
(v) And carrying out heat exchange and cooling on the water phase fluid obtained by separation in the oil-water separator, and directly sending the water phase fluid into a synthetic water treatment unit after filtering to carry out separation of oxygen-containing organic matters and purification treatment of synthetic water.
14. The method of paragraph 13, wherein the heat exchanger is a double pipe heat exchanger or a plate heat exchanger.
15. The method of paragraph 14, wherein the heat exchange means of the heat exchanger is steam or electrical heating.
Examples
The invention is further illustrated below with reference to examples, embodiments of which include, but are not limited to, the following examples.
Unless otherwise indicated, the materials, equipment, and test methods referred to in the examples below are conventional materials, equipment, and test methods known in the art.
Example 1
(1) The flow rate is 1m 3 The Fischer-Tropsch synthesis water 101 of/h is fed into a raw material water tank T1 for standing, and oil phase products 102 and water phase products 103 are obtained through separation.
(2) The water phase product 103 is fed into a heat exchanger E1 (plate heat exchanger) to be heated to 150 ℃ by a feed pump P1, and an oil removal system adopts N 2 Back pressure of 2.4MPa, mixing the aqueous product 103 with a fischer-tropsch heavy wax (distillation range temperature of about 300 ℃ to about 700 ℃, ibp=about 300 ℃, fbp=about 700 ℃,50% distillation temperature of about 550 ℃, carbon number distribution of C9 to C77) in a volume ratio of 1:1 in a static mixer M1 to obtain a mixed liquid 105.
(3) The mixed solution 105 was fed to an oil-water separator T2, and oil-water separation was performed at a temperature of 150℃and a pressure of 2.4 MPa.
(4) A part 107 of the oil phase product 106 from the oil-water separator T2 and the oil phase product 102 from the raw material water tank are mixed and output to a downstream unit, and the other part 108 of the oil phase product 106 is returned to the inlet of the static mixer M1 to be secondarily mixed with the water phase product 103, wherein the volume ratio of 107 to 108 is 1:5.
(5) The aqueous phase stream 109 (0.99 m) 3 And/h) after heat exchange and cooling to 40 ℃, filtering by a filter screen with the aperture of 5 mu m, and directly feeding into a synthetic water treatment unit for separation of oxygen-containing organic matters and purification treatment of synthetic water.
TABLE 1 Water quality index analysis of streams 101 and 109
Example 2
(1) The flow rate is 1m 3 The Fischer-Tropsch synthesis water 101 of/h is fed into a raw water tank T1 for standing, and the obtained oil phase product 102 and water phase product 103 are separated.
(2) The water phase product 103 is fed into a heat exchanger E1 (a double-pipe heat exchanger) to be heated to 220 ℃ by a feed pump P1, and an oil removal system adopts N 2 Back pressure of 2.4MPa, mixing the aqueous product 103 with a fischer-tropsch heavy wax (distillation range temperature of about 280 ℃ to about 650 ℃, ibp=about 280 ℃, fbp=about 650 ℃,50% distillation temperature of about 520 ℃ and carbon number distribution of C9 to C77) in a volume ratio of 2:1 in a static mixer M1 to obtain a mixed liquid 105.
(3) The mixed solution 105 was fed to an oil-water separator T2, and oil-water separation was performed at a temperature of 220℃and a pressure of 2.4 MPa.
(4) A part 107 of the oil phase product 106 from the oil-water separator T2 and the oil phase product 102 from the raw material water tank are mixed and output to a downstream unit, and the other part 108 of the oil phase product 106 is returned to the inlet of the static mixer M1 to be secondarily mixed with the water phase product 103, wherein the volume ratio of 107 to 108 is 1:10.
(5) The aqueous phase stream 109 (0.99 m) 3 And/h) after heat exchange and cooling to 40 ℃, filtering by a filter screen with the aperture of 1 mu m, and directly feeding into a synthetic water treatment unit for separation of oxygen-containing organic matters and purification treatment of synthetic water.
TABLE 2 Water quality index analysis of streams 101 and 109
Example 3
(1) The flow rate is 1m 3 Feeding/h Fischer-Tropsch synthesis water 101 into a raw material water tank T1, standing, and separating to obtainAn oil phase product 102 and an aqueous phase product 103.
(2) The water phase product 103 is fed into a heat exchanger E1 (a double-pipe heat exchanger) to be heated to 180 ℃ by a feed pump P1, and an oil removal system adopts N 2 Back pressure of 2.4MPa, mixing the aqueous product 103 with a fischer-tropsch heavy wax (distillation range temperature of about 280 ℃ to about 650 ℃, ibp=about 280 ℃, fbp=about 650 ℃,50% distillation temperature of about 520 ℃ and carbon number distribution of C9 to C77) in a volume ratio of 2:1 in a static mixer M1 to obtain a mixed liquid 105.
(3) The mixed solution 105 was fed to an oil-water separator T2, and oil-water separation was performed at a temperature of 180℃and a pressure of 2.0 MPa.
(4) A part 107 of the oil phase product 106 from the oil-water separator T2 and the oil phase product 102 from the raw material water tank are mixed and output to a downstream unit, and the other part 108 of the oil phase product 106 is returned to the inlet of the static mixer M1 to be secondarily mixed with the water phase product 103, wherein the volume ratio of 107 to 108 is 1:1.
(5) The aqueous phase stream 109 (0.99 m) 3 And/h) after heat exchange and cooling to 40 ℃, filtering by a filter screen with the aperture of 0.5 mu m, and directly feeding the filtered water into a synthetic water treatment unit for separation of oxygen-containing organic matters and purification treatment of synthetic water.
TABLE 3 Water quality index analysis of streams 101 and 109
Example 4
(1) The flow rate is 1m 3 The Fischer-Tropsch synthesis water 101 of/h is fed into a raw water tank T1 for standing, and the obtained oil phase product 102 and water phase product 103 are separated.
(2) The water phase product 103 is fed into a heat exchanger E1 (plate heat exchanger) to be heated to 80 ℃ by a feed pump P1, and an oil removal system adopts N 2 Back pressure of 2.4MPa, water phase product 103 and fischer-tropsch heavy oil (distillation range temperature of about 100 ℃ to about 600 ℃, ibp=about 100 ℃, fbp=about 600 ℃,50% distillation temperature of about 350 ℃, carbon number distribution of C6 to C54) are mixed according to the followingThe volume ratio of 2:1 was mixed in the static mixer M1 to obtain a mixed solution 105.
(3) The mixed solution 105 was fed to an oil-water separator T2, and oil-water separation was performed at a temperature of 80 ℃ under a slight positive pressure.
(4) A part 107 of the oil phase product 106 from the oil-water separator T2 and the oil phase product 102 from the raw material water tank are mixed and output to a downstream unit, and the other part 108 of the oil phase product 106 is returned to the inlet of the static mixer M1 to be secondarily mixed with the water phase product 103, wherein the volume ratio of 107 to 108 is 1:1.
(5) The aqueous phase stream 109 (1 m 3 And/h) after heat exchange and cooling to 40 ℃, filtering by a filter screen with the aperture of 0.1 mu m, and directly feeding the filtered water into a synthetic water treatment unit for separation of oxygen-containing organic matters and purification treatment of synthetic water.
TABLE 4 Water quality index analysis of streams 101 and 109
Comparative example 5
(1) The flow rate is 1m 3 The Fischer-Tropsch synthesis water 101 of/h is fed into a raw water tank T1 for standing, and the obtained oil phase product 102 and water phase product 103 are separated.
(2) The water phase product 103 is fed into a heat exchanger E1 (plate heat exchanger) to be heated by a feed pump P1
The deoiling system is at normal pressure at 40 ℃, the water phase product 103 and Fischer-Tropsch synthesis light oil (the distillation range temperature is about
Ibp= -40 ℃, FBP = about 300 ℃,50% distillation temperature about 200 ℃, carbon
The number distribution is C4-C30) are mixed in a static mixer M1 according to the volume ratio of 1:1 to obtain
And a mixed solution 105.
(3) Feeding the mixed solution 105 into an oil-water separator T2, and performing oil under normal pressure and 40 DEG C
And (5) separating water.
(4) A portion 107 of the oil phase product 106 from the oil-water separator T2 is combined with the feed
The oil phase product 102 from the water tank is mixed and then output to a downstream unit, and the other part of the oil phase product 106
The fraction 108 is returned to the inlet of the static mixer M1 for secondary mixing with the aqueous product 103, wherein 107
And 108 are 1:1 by volume.
(5) The aqueous phase stream 109 (1 m 3 And/h) carrying out sampling analysis.
TABLE 3 Water quality index analysis of streams 101 and 109
From the above analysis results, when oil-water mixing is performed at a lower temperature, petroleum in the aqueous phase fluid obtained after oil removal treatment increases, which means that oil-water further emulsification is caused by failure to achieve effective oil removal during the treatment involving oil-water mixing at a lower temperature, and the index of the effluent petroleum increases.
Claims (10)
1. A method for removing oil from fischer-tropsch synthesis water, comprising:
(1) Feeding the emulsified Fischer-Tropsch synthesis water into a raw material water tank for standing, and separating to obtain an oil phase product and a water phase product;
(2) Heating the water phase product to not lower than 80 ℃ by a heat exchanger, and then mixing the water phase product with oily substances to obtain mixed liquid, wherein the oily substances are Fischer-Tropsch synthesis light oil, fischer-Tropsch synthesis heavy oil and/or Fischer-Tropsch synthesis heavy wax, and the volume ratio of the water phase product to the oily substances is 1:10-10:1;
(3) Feeding the mixed solution into an oil-water separator for oil-water separation;
(4) Mixing part or all of the oil phase product from the oil-water separator with the oil phase product from the raw material water tank and outputting the mixture to a downstream unit;
(5) And carrying out heat exchange and cooling on the water phase fluid obtained by separation in the oil-water separator, and then sending the water phase fluid into a synthetic water treatment unit after filtering to carry out separation of oxygen-containing organic matters and purification treatment of synthetic water.
2. The process of claim 1 wherein in step (1) the total oxygenate content in the fischer-tropsch synthesis water is from 2wt% to 5wt%; cod=15000 to 60000mg/L; ph=2 to 4; the total oil is not higher than 10000mg/L, and petroleum is not higher than 2000mg/L.
3. The process according to claim 1 or 2, wherein in step (2) the aqueous phase product is heated to 80 ℃ to 300 ℃ via a heat exchanger;
preferably, in step (2), the mixing is performed at 1 normal atmospheric pressure or higher;
preferably, in step (2), the volume ratio of the aqueous phase product to the oily substance is from 1:5 to 5:1;
preferably, in step (2), the aqueous phase product is mixed with the oily substance using a static mixer.
4. A process according to any one of claims 1 to 3, wherein in step (3) the oil-water separator is operated at a temperature of from 80 ℃ to 300 ℃; the pressure is 0-5 MPa based on gauge pressure.
5. The process of any one of claims 1-4, wherein in step (4), a portion of the oil phase product exiting the oil-water separator may be returned to step (2) for re-mixing with the aqueous phase product, and another portion of the oil phase product exiting the oil-water separator is mixed with the oil phase product exiting the feed water tank for further processing to a downstream unit.
6. The process of claim 5 wherein the volume ratio between the oil phase product exiting the oil-water separator returned to step (2) and the oil phase product exiting the oil-water separator output to a downstream unit is from 10:1 to 1:10.
7. The method of any one of claims 1-6, wherein in step (5), the heat exchange cooling comprises cooling to room temperature or cooling to a downstream unit process temperature as required by a downstream process unit;
preferably, in the step (5), the water-phase fluid is subjected to heat exchange and temperature reduction to 20-60 ℃;
preferably, in step (5), the filtration is carried out using a filter cartridge having a pore size of not more than 10 μm.
8. The method according to any one of claims 1-7, comprising the steps of:
(i) Feeding the emulsified Fischer-Tropsch synthesis water into a raw material water tank for standing, and separating to obtain an oil phase product and a water phase product;
(ii) The water phase product is fed into a heat exchanger through a feed pump to be heated to not lower than 80 ℃, and then is mixed with oily substances in a static mixer to obtain mixed liquid, wherein the oily substances are Fischer-Tropsch synthesis light oil, fischer-Tropsch synthesis heavy oil and/or Fischer-Tropsch synthesis heavy wax, and the volume ratio of the water phase product to the oily substances is 1:10-10:1;
(iii) Feeding the mixed solution into an oil-water separator for oil-water separation;
(iv) Mixing one part of the oil phase product from the oil-water separator with the oil phase product from the raw material water tank, outputting the mixture to a downstream unit, and returning the other part of the oil phase product from the oil-water separator to an inlet of a static mixer to be mixed with the water phase product again;
(v) And carrying out heat exchange and cooling on the water phase fluid obtained by separation in the oil-water separator, and directly sending the water phase fluid into a synthetic water treatment unit after filtering to carry out separation of oxygen-containing organic matters and purification treatment of synthetic water.
9. The method of claim 8, wherein the heat exchanger is a double pipe heat exchanger or a plate heat exchanger.
10. The method of claim 9, wherein the heat exchange mode of the heat exchanger is steam or electric heating.
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