CN102021016B - Method for deacidification of alkylation reaction product - Google Patents
Method for deacidification of alkylation reaction product Download PDFInfo
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Abstract
The invention relates to a method for deacidification of an alkylation reaction product. In the method, after being subject to gravity settling, mixed emulsified liquid of the alkylation reaction product (hydrocarbon oil) and sulfuric acid passes through a component with hydrophobic modified ceramic membrane at a membrane surface speed of 0.01-5m/s for separation, and the deacidification of oil is achieved in a cross current filtration mode under the operation pressure of 0.01-0.3MPa and at the operation temperature of 0-40 DEG C. Under the push of pressure, the oil passes through the ceramic membrane, acid in the oil is trapped, and the acid content in the obtained oil is lower than 100ppm, thereby greatly reducing alkaline usage and waste water generation amount in an acid-base refine system of an alkylation technology and reducing the use of electrostatic precipitation; and the ceramic membrane surface is subject to hydrophobic modification, thus the contact angle of water droplet on the membrane surface is 70 degrees-16 degrees. The method is suitable for removal of polar liquid in various oils, has the advantages of simple process, low energy consumption, high separation precision, no environment pollution and high economic and practical value, and is easy to achieve industrial application.
Description
Technical field
The present invention relates to a kind of alkylation reaction product acid stripping method, belong to membrane sepn field.
Background technology
Motor vehicle exhaust has become the main source of China's many big cities topsoil, is seriously perplexing people's life, therefore, produces clean gasoline extremely urgent, and alkylate oil is the ideal composition of clean gasoline.The sulfuric acid process alkylation process that China adopts mostly at present, alkylation reaction product need to adopt vitriol oil washing to remove sulfuric ester, and the reactant after pickling enters settling vessel.But settling vessel can not be removed sulfuric acid completely, and particularly, in order to improve catalyzed reaction efficiency, the sulfuric acid in reactor is stirred and is treated as fine droplets, has increased settlement separate difficulty.These sulfuric acid enter subsequent technique, cause production unit heavy corrosion.At present in actual production, the normal method adopting is, by the emulsion after pickling through electrostatic precipitation, then after soda lye wash the separated sulfuric acid of removing of the mode of electrostatic precipitation.Adopt this method, can effectively remove the sulfuric acid in alkylation reaction product, but need to use a large amount of alkali and produce a large amount of waste water, simultaneous problem is that system seriously corroded and electric precipitator power transmission are undesired, and the major cause of system seriously corroded is exactly electric precipitator undesired the causing of coming into operation.Therefore be badly in need of the efficient new separation technology of exploitation.
In alkylated reaction thing, the removal of a small amount of sulfuric acid is a kind of removal of non-polar solvent system Semi-polarity drop, the existing correlative study that can use for reference both at home and abroad, and wherein oil dehydrating is more typical process.The more oil dehydrating method of current industrial use mainly contains:
(1). gravitational separation process
Be gravitational settling, its principle is to utilize the immiscible property of density difference and oily and the water of oil and water, realizes the separated of water droplet and fluid under static or low speed flow state.Gravitational settling can be removed large-size water droplet in fluid to reach the object tentatively dewatering.One use gravitational separation process of fluid that aqueous concentration is larger is processed.From service condition, the major equipment of gravitational settling has except water pot, removes pond etc., needs very large container and very low flow velocity, and the treatment time is longer.
(2). centrifugal separation
Centrifugal separation is the container high speed rotating that makes to be equipped with oil-water mixture, forms centrifuge field and realizes oily water separation, and common equipment is cyclone separator.Cyclone separator originates from Britain, and early stage bicone cyclone separator develops into now and has identical separation performance with bicone but treatment capacity will exceed the tapered cyclone separator of list of a times.Also, at numerous and confused research centrifuge separator, for the higher mixed system of water content, there is good effect in domestic a lot of R&D institution, but while disperseing for water content less system, especially water droplet, treatment effect is undesirable.
(3). vacuum hydro-extraction
Vacuum hydro-extraction refers to because oil is different with the boiling point of water, can make by the method for vacuum distilling the two separation.This method can be removed free water, emulsified water and dissolved water, can remove the whole water in fluid, but need to fluid be heated to the boiling point of water under this pressure under vacuum, so energy consumption is very high.One capacity of the equipment of vacuum hydro-extraction is less, and processing efficiency is lower.
(4). chemical demulsification method
Chemical dehydration adds some macromolecular organic compound exactly in oil product, this material can be adsorbed in an oily water termination, reduce the physical strength of interfacial film, change emulsion type, destroy the stability of emulsion, make small droplets be merged into larger drop, this kind of material is commonly called emulsion splitter.Chemical demulsification method removes moisture in oil product, owing to adding chemical agent, can in oil product, introduce new impurity.Because chemical demulsifier has very high surfactivity, may cause follow-up sewage disposal difficulty.Therefore need the new emulsion splitter of the friendly type of development environment.
(5). ultrasonic separation method
Ultrasonication oil-water mixture can produce cohesion, hole or cavitation effect in mixed solution.When ultrasonic wave is passed through mixed solution, can cause the vibration of small water droplet.Because the particle varying in size has different Relative Vibration speed, water droplet will collide mutually, bonding, and the volume of water droplet increases gradually.Water droplet after increase can sink by gravity, reaches separated object.For a large amount of oil-water mixtures, directly use ultrasonic wave separating effect not good, one need to be combined with other separation methods.
(6). EDN
The ultimate principle of oil product electro-dewatering is: to the oil product extra electric field in encloses container, make the globule polarization in oil emulsion, become electric dipole, electric dipole attracts each other, make droplet aggregate into the larger globule, sedimentation under action of gravity and separated with oil product.But, high-voltage field removes moisture in oil product, while processing the higher oil emulsion of water content, understand the strength of electric field that produces electrical breakdown and cannot set up interpolar necessity, so the de-method of electricity is not suitable for independent use, the best post-order process as other treatment process, and the de-method energy consumption of electricity is large, and the residence time is long.
By above various methodologies, can be found out, conventional oil dehydrating method has its distinctive advantage, and as simple in equipment, less investment, dehydrating effect are good etc., still also exist more outstanding shortcoming.
Along with the pay attention to day by day of people to environment protection, oil dehydrating need to lower pollution, few energy consumption, easy-operating method.And membrane separation technique relies on, hold facility volume is little, simple to operate, low power consumption and other advantages is applied to every field more and more widely.
Membrane separation process carries out oil dehydrating, is lipophilicity or the wetting ability of utilizing porous membrane, by screening, film phase-splitting, reverse osmosis or super penetration theory, the oil in liquid/liquid dispersion system and water is separated.If the precision that dewaters requiring is high, can also utilize more high-precision film that dissolved water is removed.
Chinese patent CN101530680A has announced the method for utilizing hydrophobic organic membrane to carry out oil dehydrating.The filtering traffic of this method is 10ml/min～500ml/min, and moisture rejection can reach more than 99%, and hydrophobic membrane can reach 2～5 months work-ing life.The method energy consumption is low, and dehydration rate is high, but the life-span of hydrophobic organic membrane is shorter, needs periodic replacement.
(the Ezzati A such as Ezzati, Gorouhi E, Mohammadi T.Separation of water in oilemulsions using microfiltration[J] Desalination, 2005,185:371-38.) with aperture, be water/gasoline system of the hydrophobic PTFE membrane sepn water content 5-20% of 0.45 μ m, under optimal conditions, the permeation flux obtaining is 40L/m
2.h, the rejection of water is reached to 95%.(the Hu B such as Hu, Scott K.Microfiltration of water in oil emulsions and evaluation of fouling mechanism[J] Chem Eng J, 2008,136:210-220.) employing aperture is water/kerosene system that the hydrophobic PTFE membrane sepn water content of 0.2 μ m is 30%, at transmembrane pressure, be 0.6bar, crossflow velocity is under 1.5m/s, and obtaining steady seepage flux is 20L/m
2h.The hydrophobic PTFE film that these two kinds of methods are used, have too the problem that need to regularly replace film, and the steady seepage flux of gained is also lower.
The advantages such as and ceramic membrane is good because having chemical stability, physical strength is large, and anti-microbe ability is strong, have been applied in oily water separation field more and more.
The people such as Zeng Jianxian (Zeng Jianxian, Zheng Lifeng. experimental study [J] the process engineering journal of ceramic membrane purifying solvent oil, 2010,10:488～492) employing mean pore size is that the solvent oil that the ceramic membrane of 0.2 μ m is 0.5wt% to water content carries out micro-filtration separation, has investigated operating time, transmembrane pressure, cross-flow velocity, the impact of temperature on membrane flux and aluminium powder rejection.Under suitable operating conditions, the film stabilized flux obtaining is 144.5L/ (m
2h).The resulting membrane flux of this method is also little, and exists more serious film to pollute with this method purifying solvent oil, needs recoil and solvent cleaning to recover membrane flux.
Summary of the invention
The object of the invention is to solve the problems such as the corrosion of system in existing alkylation reaction product depickling technology and settling vessel be unstable, a kind of efficient, environmental protection, energy-conservation alkylation reaction product acid stripping method are provided.
Technical scheme of the present invention is: membrane separation process principle of the present invention is: the ceramic membrane surface oleophilic drainage of hydrophobically modified, under the promotion of pressure difference, when the ceramic membrane of use modification removes the sulfuric acid in alkylation reaction product, oil is because of the strong avidity on itself and oleophilic drainage surface, preferentially by film, arrive per-meate side, and the sulfuric acid droplets of polarity can not soak the ceramic membrane surface of hydrophobically modified, and within the scope of emergent pressure, sulfuric acid droplets can not permeation ceramic membrane, therefore be trapped.
Concrete technical scheme of the present invention is: a kind of method of alkylation reaction product depickling, its concrete steps are as follows: the mix emulsion fluid of alkylation reaction product and sulfuric acid is through gravity settling after 1～6 hour, by infusion, enter to be equipped with in the membrane module of modified ceramic film, adjustment operation temperature, at 0 ℃～40 ℃, adopts cross flow filter mode to filter; In the oil obtaining, acid content is lower than 100ppm; Oil after processing enters subsequent disposal, realizes the removal completely of sulfuric acid; Wherein said modified ceramic film is surperficial oleophilic drainage, and the contact angle of water droplet on film surface is 70 °～160 °.
Alkylation reaction product of the present invention is the mixture of multiple hydrocarbon-type oil.One is 5～70wt% for acid solution content in mix emulsion fluid.
Gravity settling operation of the present invention is standing sedimentation, and oil and acid, by the immiscible property of density difference and oil and acid, realize initial gross separation.In oil after gravity settling, acid content is 0.5～10wt%.
During cross flow filter, control crossflow velocity is 0.01～5m/s, controls transmembrane pressure at 0.01～0.3Mpa.
The separating layer of the ceramic membrane of surface modification of the present invention is at least a kind of in aluminum oxide, zirconium white, titanium oxide or silicon oxide.The mean pore size of the ceramic membrane of surface modification is 0.01～1.4 μ m.
The surface modification of ceramic membrane of the present invention is to pass through chemical process, at organism such as ceramic membrane surface grafting organochlorosilane, methoxy silane, concrete method of modifying is with reference to the inventor patent CN101280241A in early stage, and the contact angle on the film surface of water droplet after modification is 70 °～160 °.
In the oil product of gained of the present invention, acid content is lower than 100ppm, greatly reduced the consumption of alkali and the generation of waste water in the acid-alkali refining system of alkylation process, and reduced the use of electrostatic precipitation.
Service temperature of the present invention one at 0 ℃～40 ℃, applicable too for the feed liquid of higher temperature.
Concentrated solution after ceramic membrane filter of the present invention turns back in settling bowl, has realized the separated of sulfuric acid and alkylation reaction product and has collected.
The subsequent disposal operation of per-meate side oil of the present invention is the minute quantity sulfuric acid except the middle dissolving of deoiling, and can be the methods such as soda lye wash.
Technique of the present invention also can be for other the subtractive process of oil product Semi-polarity drop, as: the stock oil acid number of biodiesel synthesis is higher, removes the acid in stock oil oil; Removal of water or sour water etc. in synthetic oil technique.
Beneficial effect:
(1) the present invention does not use the operations such as centrifugal, electrostatic precipitation, distillation, has saved largely energy consumption.
(2) it is good that the ceramic membrane that the present invention uses has ceramic membrane chemical stability, and physical strength is large, and the advantages such as anti-microbe ability is strong, long service life, are green friendly economic parting materials.
(3) the present invention carries out chemical modification to ceramic membrane surface, makes ceramic membrane surface have hydrophobic lipophilicity, is beneficial to oily infiltration and the interception of acid solution.
(4) separation accuracy of the present invention is high, and in the oil after processing, acid content, lower than 100ppm, has greatly reduced the consumption of alkali and the generation of waste water in the acid-alkali refining system of alkylation process, has reduced the use of electrostatic precipitation.
(5) the present invention is simple to operate, less investment, and practical value is high.
Accompanying drawing explanation
Fig. 1 is that the present invention carries out the cross flow filter process flow sheet of oil dehydrating with ceramic membrane; 1-settling bowl wherein, 2-charging stock tank, 3-fresh feed pump, 4,8-variable valve, 5,7-tensimeter, 6-ceramic film component, 9-spinner-type flowmeter, 10-tapping valve, A-subsequent disposal.
Embodiment
The present invention is described in detail below to use specific embodiment, but do not limit use range of the present invention.
Embodiment 1
Adopt the process flow sheet shown in Fig. 1.
Selecting supporting layer is Alpha-alumina, and separating layer is zirconic tubular ceramic membrane, and mean pore size is 0.05 μ m, adopts the modification of hexadecyl Trimethoxy silane.Concrete method of modifying is: ceramic membrane is soaked in the ethanol that is dissolved with hexadecyl Trimethoxy silane after 4 hours, with ethanol, repeatedly clean 5 times, finally in baking oven, at 120 ℃, be dried 3 hours, water droplet ceramic membrane surface contact angle after modification is 140 °.
Use alkylation reaction product acid stripping method of the present invention, separating oil/sulfuric acid mix emulsion fluid.By 5L mix emulsion fluid, after standing 4 hours, supernatant liquid is poured in charging stock tank; Use pump the oil in charging stock tank/sulfuric acid mixture liquid to be injected to the membrane module that surface modification ceramic membrane is housed, service temperature is 30 ℃, regulated valve 4 and 8 aperture, making manometric average reading is that transmembrane pressure is 0.1MPa, the reading of spinner-type flowmeter is 5L/min, be that crossflow velocity is 1.67m/s, carry out cross flow filter; After experiment finishes, open valve, feed liquid is discharged and collected in the container for storing liquid of sealing.It is 1938L/ (m that experiment records steady seepage flux
2h), per-meate side acid content is 95ppm.Oil after ceramic membrane is processed adopts soda lye wash again, and acid content is 5ppm.
Embodiment 2
Adopt the process flow sheet shown in Fig. 1.
Petrochemical plant can produce a large amount of vitriolated waste oil in process of production, and the main component in these waste oil is oil, but owing to containing a large amount of sulfuric acid, cannot directly use.If sulfuric acid composition wherein can be removed, remaining oil composition wherein still can be used.
Use alkylation reaction product acid stripping method of the present invention, separate sulphur acid oil, selecting supporting layer is beta-alumina, separating layer is the tubular ceramic membrane of aluminum oxide, mean pore size is 0.2 μ m, adopt the modification of octadecyl trichlorosilane alkane, all the other modification procedure are with embodiment 1, and water droplet ceramic membrane surface contact angle after modification is 130 °; Service temperature is 40 ℃, and other operate with embodiment 1.The steady seepage flux obtaining is 1080L/ (m
2h), in per-meate side oil, acid content is 90ppm.Oil after ceramic membrane is processed adopts soda lye wash again, and acid content is 7ppm.
Embodiment 3
Adopt the process flow sheet shown in Fig. 1.
In production of propylene oxide, can produce a large amount of waste oil, current waste oil tripping device often can cause acid water to enter waste oil groove, thereby has affected the quality of waste oil product and strengthened the extent of corrosion of pipeline, equipment.
Use alkylation reaction product acid stripping method of the present invention, the separated production of propylene oxide waste oil containing sour water, selecting supporting layer is Alpha-alumina, separating layer is the tubular ceramic membrane of titanium oxide, mean pore size is 0.05 μ m, adopts the modification of normal-butyl dimethylchlorosilane, soaks 10 hours, all the other modification procedure are with embodiment 1, and water droplet ceramic membrane surface contact angle after modification is 95 °; Working pressure is 0.03MPa, and feed liquid flow is 0.3L/min, and crossflow velocity is 0.1m/s, and other operate with embodiment 1.The steady seepage flux obtaining is 600L/ (m
2h), in per-meate side waste oil, sour water content is 30ppm.Oil after ceramic membrane is processed adopts soda lye wash again, and acid content is 8ppm.
Embodiment 4
Adopt the process flow sheet shown in Fig. 1.
Refinery adopts caustic washing electric refining technique to fraction oil deacidification more, but this method investment and process cost are high, and waste lye quantity discharged is high.
Use alkylation reaction product acid stripping method of the present invention, separated refinery distillate, selecting supporting layer is Alpha-alumina, separating layer is the tubular ceramic membrane of aluminum oxide, mean pore size is 0.05 μ m, adopts the modification of hexadecyl Trimethoxy silane, soaks 6 hours, all the other modification procedure are with embodiment 1, and water droplet ceramic membrane surface contact angle after modification is 135 °; Working pressure is 0.15MPa, and other operate with embodiment 1.The steady seepage flux obtaining is 1220L/ (m
2h), per-meate side sour water content is 88ppm.Oil after ceramic membrane is processed adopts soda lye wash again, and acid content is 10ppm.
Embodiment 5
Adopt the process flow sheet shown in Fig. 1.
In widely used ester-interchange method biodiesel synthesis technique, the existence of water can impel fat hydrolysis and generate soap with alkali, therefore, take mineral alkali during as catalyzer, usually requires in stock oil (as plant wet goods) moisture lower than 0.06%.
Use alkylation reaction product acid stripping method of the present invention, remove the moisture in vegetables oil, selecting supporting layer is Alpha-alumina, separating layer is zirconic tubular ceramic membrane, mean pore size is 0.2 μ m, adopts trimethylchlorosilane modification, soaks 6 hours, all the other modification procedure are with embodiment 1, and water droplet ceramic membrane surface contact angle after modification is 130 °; Other operations are with embodiment 1.The steady seepage flux obtaining is 1420L/ (m
2h), in per-meate side vegetables oil, water-content is 75ppm.
Embodiment 6
Adopt the process flow sheet shown in Fig. 1.
Engine oil is in the continuous working cycle of oiling system; the effective constituent of self can constantly be consumed; also have some foreign matters simultaneously and sneak into as moisture, fuel oil, sand-dust impurity etc., the use properties of machine oil will decline like this, even loses the protectiveness to engine.While containing excess water in machine oil, the use properties of machine oil will decline, excessive moisture can make portions additive use properties in machine oil reduce even inefficacy under certain condition, meeting destruction machine oil viscosity, make machine oil in motion friction fit pair, form good oil-bound film, thereby make machinery produce inordinate wear, even cause mechanical fault.
Use alkylation reaction product acid stripping method of the present invention, separated moisture engine motor oil, selecting supporting layer is Alpha-alumina, separating layer is the tubular ceramic membrane of silicon oxide, mean pore size is 0.1 μ m, adopt the modification of octyl group trichlorosilane, all the other modification procedure are with embodiment 1, and water droplet ceramic membrane surface contact angle after modification is 130 °; Working pressure is 0.08MPa, and feed liquid flow is 0.6L/min, and crossflow velocity is 0.2m/s, and other operate with embodiment 1.The steady seepage flux obtaining is 1100L/ (m
2h), in per-meate side machine oil, water-content is 70ppm.
Embodiment 7
Adopt the process flow sheet shown in Fig. 1.
In the used oil pipe of hydraulic efficiency installation, oily-water seperating equipment is installed, the moisture in oil return and oil content are opened in time and drained, to preventing oil emulsion, extend oil product significant work-ing life.
Use alkylation reaction product acid stripping method of the present invention, separated aqueous fluid force feed, select supporting layer and separating layer to be zirconic tubular ceramic membrane, mean pore size is 0.2 μ m, adopt trimethylchlorosilane modification, soak 7 hours, all the other modification procedure are with embodiment 1, and water droplet ceramic membrane surface contact angle after modification is 105 °; Service temperature is that working pressure is 0.05MPa, and feed liquid flow is 0.1L/min, and crossflow velocity is 0.033m/s, and other operate with embodiment 1.The steady seepage flux obtaining is 800L/ (m
2h), per-meate side W/O content is 60ppm.
Embodiment 8
Adopt the process flow sheet shown in Fig. 1.
The oil product of service station, through long-distance transport, and pours in the process of service station's oil reservoir, can mix the water of part in fuel oil, and quality of gasoline is declined, can not perfect combustion, easily there is engine knock and engine knock phenomenon.Therefore, gasoline needs purifying treatment before using.
Use alkylation reaction product acid stripping method of the present invention, separated moisture 93# gasoline, selecting supporting layer is Alpha-alumina, separating layer is zirconic tubular ceramic membrane, mean pore size is 0.02 μ m, adopts KH570 modification, soaks 10 hours, all the other modification procedure are with embodiment 1, and water droplet ceramic membrane surface contact angle after modification is 105 °; Working pressure is 0.2MPa, and other operate with embodiment 1.The steady seepage flux obtaining is 950L/ (m
2h), in per-meate side gasoline, water-content is 65ppm.
Claims (1)
1. the method for an alkylation reaction product depickling, its concrete steps are as follows: the mix emulsion fluid of alkylation reaction product and sulfuric acid is through gravity settling after 1～6 hour, by infusion, enter to be equipped with in the membrane module that mean pore size is 0.01～1.4 μ m modified ceramic film, adjustment operation temperature is at 0 ℃～40 ℃, adopt cross flow filter mode to filter, control crossflow velocity is 0.01～5m/s, controls transmembrane pressure at 0.01～0.3Mpa; In the oil obtaining, acid content is lower than 100ppm; Oil after processing enters subsequent disposal, realizes the removal completely of sulfuric acid; Wherein said modified ceramic film is to pass through chemical process, at ceramic membrane surface grafting organism, the contact angle on the film surface of water droplet after modification is 70 °～160 °, and the separating layer of the ceramic membrane of surface modification is at least a kind of in aluminum oxide, zirconium white, titanium oxide or silicon oxide.
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| CN102229850B (en) * | 2011-06-08 | 2013-05-08 | 南京工业大学 | Waste hydraulic oil regenerating method and equipment |
| CN104857742B (en) * | 2015-05-28 | 2017-05-31 | 重庆理工大学 | A kind of water-eliminating method of dichloromethane |
| CN105670686B (en) * | 2016-03-04 | 2017-09-12 | 华东理工大学 | The method and apparatus of alkylated reaction effluent pickling |
| CN108070401B (en) * | 2016-11-15 | 2020-03-17 | 中国石油化工股份有限公司 | Separation method of alkylation reaction product |
| CN108070400B (en) * | 2016-11-15 | 2020-03-17 | 中国石油化工股份有限公司 | Alkylation method |
| CN106861436A (en) * | 2017-03-16 | 2017-06-20 | 安阳工学院 | One kind is using nano ceramics hyperfiltration treatment alkylation spent acid technique |
| CN109485192A (en) * | 2017-09-12 | 2019-03-19 | 江苏赛瑞迈科新材料有限公司 | It is alkylated spent acid ceramic membrane filter device |
| CN115364670B (en) * | 2021-05-21 | 2024-04-19 | 三达膜科技（厦门）有限公司 | Preparation method of oil-water separation modified spherical alumina ceramic microfiltration membrane |
| CN114588844B (en) * | 2022-03-18 | 2023-07-21 | 杭州师范大学 | Application of double-sided hollow fiber membrane reactor in Suzuki-Miyaura reaction and membrane reactor thereof |
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| US4411790A (en) * | 1980-05-22 | 1983-10-25 | Commissariat A L'energie Atomique | Process for the treatment of a hydrocarbon charge by high temperature ultrafiltration |
| CN101070507A (en) * | 2007-06-05 | 2007-11-14 | 天津新膜科技有限责任公司 | Regeneration method for waste lubricant and apparatus |
| CN101280241A (en) * | 2008-05-22 | 2008-10-08 | 南京工业大学 | Method for purifying waste lubricant oil |
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| US4411790A (en) * | 1980-05-22 | 1983-10-25 | Commissariat A L'energie Atomique | Process for the treatment of a hydrocarbon charge by high temperature ultrafiltration |
| CN101070507A (en) * | 2007-06-05 | 2007-11-14 | 天津新膜科技有限责任公司 | Regeneration method for waste lubricant and apparatus |
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