CN105540900A - Method and device for treating alkylated waste acid and recovering organic phase - Google Patents
Method and device for treating alkylated waste acid and recovering organic phase Download PDFInfo
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- CN105540900A CN105540900A CN201610120430.6A CN201610120430A CN105540900A CN 105540900 A CN105540900 A CN 105540900A CN 201610120430 A CN201610120430 A CN 201610120430A CN 105540900 A CN105540900 A CN 105540900A
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- spent acid
- acid
- emulsion
- organic phase
- alkylation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- 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
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- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
Abstract
The invention relates to a method and a device for treating alkylated waste acid and recovering an organic phase and provides the method for treating the alkylated waste acid and recovering the organic phase. The method comprises steps as follows: a, the waste acid produced through sulfuric acid alkylation is subjected to sedimentation and coarse separation treatment; b, the waste acid subjected to the sedimentation and coarse separation treatment is subjected to mechanical demulsification treatment; c, the waste acid after mechanical demulsification treatment is subjected to oil-acid two-phase separation, an obtained oil phase returns to an alkylation system, and the waste acid is discharged to the downstream for treatment. The invention further provides the device for treating the alkylated waste acid and recovering the organic phase.
Description
Technical field
The invention belongs to alkylation spent acid process field, relate to the method and apparatus of a kind of waste sulfuric acid from alkylation process and organic phase recycling.
Background technology
Current, the topsoil situation of China is very severe, becomes increasingly conspicuous with the regional atmospheric environment problem that pellet (PM10), fine particle (PM2.5) are characteristic contamination.In May, 2015; seven departments such as National Development and Reform Committee, the Ministry of Finance, Environmental Protection Department combine and print and distribute " accelerating processed oil quality upgrading programme of work ", and the major objective of scheme determines automobile-used vapour, the diesel oil of state of enforcement V standard in China before 1 day January in 2017.Comprehensive upgrading work of petrol and diesel oil is very urgent, and this just requires that oil refining enterprise accelerates upgrading paces, improves clear gusoline manufacture and development ability, and comprehensive difficulty action accomplishment upgrading task, fulfils oil refining industry prevention and control of air pollution action target responsibility in advance.Alkylation process is the alkylate oil utilizing the alkylated reaction of isobutyl institute and alkene warp to obtain, it mainly consists of C8 isoparaffin, not containing alkene, aromatic hydrocarbons and sulphur, there is the advantage of high-octane rating and low-steam pressure, in " accelerating processed oil quality upgrading programme of work ", building alkyl plant is one of emphasis direction of following gasoline upgrading.
In alkylation process, factory often adopts sulfuric acid to make catalyzer, but the waste sulfuric acid solution of a large amount of oil-containing can be produced in sulfuric acid alkylation art production process, this Waste Sulfuric Acid is the colloidal liquid that a kind of viscosity is larger, its color and luster is dark red, character is unstable, distributes singularity stink, is difficult to process, as direct discharge, severe contamination will be brought to ecotope.At present, the waste sulfuric acid from alkylation process of batch production has two kinds of techniques, and the first produces white carbon black and oil sanitas technique, the advantage of this technique: one be to spent acid process comparatively thoroughly, utilization ratio is high; But technical maturity, succeed at Jingmen refinery middle-scale device; Three is that medium and the operational condition of other supply and demand all comparatively relax except initial sedimentation divides oily gained dilute sulphuric acid to be that strong corrosive medium need with except special substance equipment.The weak point of this technique: one is that the product white carbon black market requirement is little, for the alkyl plant of low processing capacity or feasible, but for large-scale alkyl plant, produces a large amount of white carbon blacks and waits to develop the larger market requirement; Two is that this operational path is complicated, and need more equipment, solid phase prod easily blocks on equipment, pipeline; Three is that sodium silicate raw material is difficult to obtain; Four are oil sanitass of exploitation is a kind of product innovations, needs development and sale market; Five be produce in produce dilute sulphuric acid and waste liquid as directly discharge pollute the environment, need process up to standard after could discharge.The second is cracking industrial sulphuric acid, and this mature technology, required fuel refinery can conveniently provide, to useless acid-treated more thorough.But spent acid industrial sulphuric acid technique main drawback is that refinery does not have vitriolization device, and adopt this technique need increase supporting sulfuric acid production plant, separately this long flow path, equipment is many, control complicated, one-time investment strengthens; Two is that running cost is high, and device consumes a large amount of fuel gas and electric power every year, and energy consumption is many, required catalyzer price; Three is that environmental protection pressure is large, and the sulfur dioxide concentration of this operational path smoke stack emission is about 760mg/Nm
3, as met the emission concentration limit value 400mg/Nm of sulfur dioxide pollution thing
3specified requirement, newly-builtly a set ofly must schedule to last refining plant, as the ammonia process of desulfurization, alkali desulphurization etc., this just more increases the gross investment of device.
In sulfuric acid process alkylation process, alkyl plant year discharge about 20,000 tons, the spent acid of 200000 tons/year, and the organism containing 10-30% in these spent acid, organic principal monomer is polymer alkene, diolefine, polymkeric substance and alkylsulphonic acid, sulfuric ester etc., in the price of organism about 5000 yuan/ton, Organic Materials of Spent acid be lost in 1,000 ten thousand yuan/year to 3,000 ten thousand yuan/year, lose larger.Therefore, the organic phase in alkylation spent acid has larger recycling and is worth.In conventional alkylation spent acid, organic phase recovery method can adopt general subsidence style, namely adopts the gravity difference of oleic acid two-phase, makes oil phase be distributed in slurry tank upper strata, realizes recycling it.But this kind of method is comparatively simple, particularly in slurry tank lower floor spent acid, also can there is a large amount of water-in-oil/oil-in-water emulsions, and make oleic acid be separated and become more difficult, separation efficiency is low, weak effect.
In current and future time, alkylation upgrading petrol and diesel oil will become the important directions of China's oil refining industry, but alkylation spent acid difficult treatment, organic phase wherein also has larger recycling and is worth, therefore, this area in the urgent need to developing a kind of novel method, new device realizes the recycling of effective process to alkylation spent acid and organic phase.
Summary of the invention
The invention provides a kind of alkylation spent acid process of novelty and the method and apparatus of organic phase recovery, thus solve problems of the prior art.
On the one hand, the invention provides the method for the process of a kind of alkylation spent acid and organic phase recovery, the method comprises the following steps:
A. the spent acid that sulfuric acid alkylation produces is carried out sedimentation rough segmentation process;
B. the spent acid through sedimentation rough segmentation process is carried out mechanical breakdown of emulsion process;
C. the spent acid after mechanical breakdown of emulsion process is carried out oleic acid two-phase laminated flow, the oil phase of gained returns alkylation system, and the spent acid of gained enters downstream processing.
In one preferred embodiment, in described step a, use gravity settling or silk screen foam removal to carry out sedimentation rough segmentation process, the settling time is 0-2 hour.
Another preferred embodiment in, in described step a, the acid concentration of described spent acid is lower than 91%, and the organic phase content in spent acid is 10-30%.
Another preferred embodiment in, in described step c, the spent acid of gained enters downstream and carries out burning disposal.
On the other hand, the invention provides the device of the process of a kind of alkylation spent acid and organic phase recovery, this device comprises:
Spent acid for being produced by sulfuric acid alkylation carries out the slurry tank of sedimentation rough segmentation process, and it comprises an entrance and spent acid outlet;
Tank connected with sedimentation, for the spent acid through sedimentation rough segmentation process being carried out Taylor's emulsion treater of mechanical breakdown of emulsion process, it comprises a tangential inlet and a lower part outlet; And
Be connected with Taylor's emulsion treater, for the spent acid after mechanical breakdown of emulsion process being carried out the fiber capturing equipment of oleic acid two-phase laminated flow, it comprises an entrance, a light phase export and a heavy out, and this entrance is connected with the lower part outlet of Taylor's emulsion treater.
In one preferred embodiment, this device also comprises: alkylation system, and it comprises entrance and spent acid outlet; And impeller pump, it comprises a spent acid entrance and spent acid outlet, wherein, the entrance of described slurry tank exports with the spent acid of alkylation system and is connected, the spent acid outlet of described slurry tank is connected with the spent acid entrance of impeller pump, the tangential inlet of described Taylor's emulsion treater exports with the spent acid of impeller pump and is connected, and the described light phase export of fiber capturing equipment is connected with the entrance of alkylation system.
Another preferred embodiment in, described Taylor's emulsion treater is double-barrel structure, and spent acid enters urceolus through tangential inlet, and urceolus is static, motor drive inner cylinder rotating; Urceolus length is L
1, inner core length is L
2, outer barrel diameter is D
1, inner diameter of steel flue is D
2, wherein L
1=1D
1~ 3D
1, D
2=0.5D
1~ 0.9D
1, L
2=0.5L
1~ 0.8L
1; Outer tube inner wall is provided with 0-5 layer baffle plate, and barrier width is B, and length is L
0, be highly H, wherein H=1L
0~ 5L
0, L
0=1B ~ 3B; The baffle plate that outer tube inner wall every layer is arranged is 0-16, and outer tube inner wall distributes symmetrically and evenly.
Another preferred embodiment in, the pressure of described Taylor's emulsion treater reduces to 0-50KPa, and entrance flow velocity is 1-30m/s; When inner core high speed rotating, spent acid can form Taylor vortex flow between inner/outer tube, utilizes the shearing force between drop and impact force to realize breakdown of emulsion, makes organic phase agglomeration.
Another preferred embodiment in, described fiber capturing equipment is made up of shell and fiber capturing layer, wherein, fiber capturing layer by fine-fibered weave form, the diameter of fiber is 10-200um.
Another preferred embodiment in, the material of described fiber capturing layer is organic materials or metallic substance, and organic materials and metallic substance can be used alone or mixed weaving uses; Described fine-fibered has hydrophilic or lipophilicity, and when oleic acid two-phase is passed through, oleophylic fine-fibered catches thin organic phase, makes organic phase agglomeration become larger oil droplet, accelerates oleic acid two-phase laminated flow.
Accompanying drawing explanation
Fig. 1 is alkylation spent acid process according to an embodiment of the invention and organic phase recovery process schema.
Fig. 2 A is the diagrammatic cross-section of the Taylor's emulsion treater according to an embodiment of the invention.
Fig. 2 B is the diagrammatic cross-section along the structure of A-A line in Fig. 2 A.
Embodiment
Present inventor is through extensive and deep research, have to recycle for the alkylation spent acid organic phase be difficult in process and spent acid and be worth this situation, in conjunction with prior art, by sedimentation rough segmentation, machinery breakdown of emulsion, fiber capturing, the modes such as oleic acid separation, effectively solve alkylation spent acid emulsion difficult, the problems such as organic phase organic efficiency is low, propose a kind of alkylation spent acid process of novelty and the method and apparatus of organic phase recovery, realize the process of alkylation spent acid and the recycling of organic phase, the method and appliance arrangement simple, easy to operate, cost is low, pollution-free, separation efficiency is high, recovering effect is good, economic benefits.
Technical conceive of the present invention is as follows:
Spent acid after alkylated reaction is passed into slurry tank roughing out, spent acid after rough segmentation first carries out mechanical breakdown of emulsion, then passes into fiber capturing equipment and carry out oleic acid separation, and good separating effect, efficiency are high, afterwards the oil phase of gained is returned alkylation system, and the spent acid after process enters downstream process.
In a first aspect of the present invention, provide the method for the process of a kind of alkylation spent acid and organic phase recovery, the method comprises the following steps:
A. Taylor's emulsion treater is pumped into after the spent acid that sulfuric acid alkylation produces being carried out sedimentation rough segmentation process in slurry tank;
B. use Taylor's emulsion treater to carry out mechanical breakdown of emulsion process to spent acid, realize the agglomeration of organic phase; And
C. the spent acid after breakdown of emulsion is passed into fiber capturing equipment, realize oleic acid two-phase laminated flow, oil phase returns alkylation system, and spent acid enters downstream processing.
In the present invention, in described step a, the raw material of sulfuric acid alkylation is alkanes or hydro carbons, and the concentration of catalyst sulfuric acid is 86%-99%.In order to the alkane concentration ensureing in sulfuric acid needs the sulfuric acid using high density, therefore when the sulfuric acid concentration after alkylation recycles lower than 91% time need more to renew sulfuric acid, now in spent acid, the content of organic phase is 10-30%.
In the present invention, the subsidence style that the slurry tank in described step a adopts is gravity settling or silk screen foam removal mode, and slurry tank mainly plays the effect of oleic acid rough segmentation, and equipment volume is comparatively large, and disengaging time is longer, and the settling time is generally 0-2 hour.
In the present invention, the Taylor's emulsion treater in described step b is double-barrel structure, and spent acid enters urceolus through tangential inlet, and motor drives inner core high speed rotating.The necessity of breakdown of emulsion is, because sulfuric acid viscosity is large, the little oil droplet of organic phase can be enclosed in wherein and cannot shake off out, forms a large amount of water-in-oil/oil-in-water emulsions, further oleic acid will be made to be separated and become very difficult.Normal employing eddy flow machinery breakdown of emulsion or interpolation emulsion splitter, but the eddy flow residence time is shorter, undesirable for this kind of complicated emulsion system treatment effect.Add emulsion splitter, not only increase processing cost, and likely cause secondary pollution, follow-up separating-purifying workload is also larger.
In the present invention, the urceolus length L of described Taylor's emulsion treater
1, inner core length L
2, outer barrel diameter D
1, inner diameter of steel flue D
2, wherein L
1=1D
1~ 3D
1, D
2=0.5D
1~ 0.9D
1, L
2=0.5L
1~ 0.8L
1.The outer tube inner wall of described Taylor's emulsion treater is provided with 0-5 layer baffle plate, barrier width B, length L
0, height H, wherein H=1L
0~ 5L
0, L
0=1B ~ 3B.
In the present invention, the baffle plate that the outer tube inner wall every layer of described Taylor's emulsion treater is arranged is 0-16, and outer tube inner wall distributes symmetrically and evenly.
In the present invention, the pressure of described Taylor's emulsion treater reduces to 0-50KPa, and entrance flow velocity is 1-30m/s.Keep higher entrance flow velocity can increase the residence time of spent acid in Taylor's emulsion treater as much as possible, maintain good demulsification, further, higher entrance flow velocity does not need motor to provide too many energy to start the circling behavior that spent acid follows inner core, and energy waste is less.
In the present invention, the mechanism of the mechanical breakdown of emulsion in described Taylor's emulsion treater is: when inner core high speed rotating, spent acid can form Taylor vortex flow between inner/outer tube, utilizes the shearing force between drop and impact force to realize breakdown of emulsion, makes organic phase agglomeration.
In the present invention, the Taylor's emulsion treater in described step b can according to processing power requirement, and separate unit or multiple stage parallel connection use; Or according to separation accuracy requirement, separate unit or multiple stage series connection use.When used in series, suitably impeller pump to be increased at Taylor's emulsion treater place of being interconnected, to maintain inlet pressure and entrance flow velocity according to pressure loss.
In the present invention, the fiber capturing equipment in described step c is made up of shell and fiber capturing layer, and fiber capturing layer is that fine-fibered braiding forms, and the diameter of fiber is 10-200um.Organic phase particle diameter is little, particle size range 10-50um, adopts fine-fibered can catch thin organic phase.
In the present invention, the fiber capturing layer in the fiber capturing equipment in described step c is organic materials or metallic substance, or the mixed weaving thing of bi-material, and per-cent during mixed weaving shared by differing materials by mass.Organic materials can adopt tetrafluoroethylene or polypropylene etc., and metallic substance can be 304 stainless steels or modification steel wire.
In the present invention, the fine-fibered of the fiber capturing equipment in described step c has hydrophilic or lipophilicity, when oleic acid two-phase is passed through, oleophylic or hydrophilic fine-fibered catch thin organic phase or aqueous phase, organic phase or aqueous phase agglomeration is made to become larger oil droplet or large water droplet, come off under the effect of liquid-flow drag force, and float due to self gravitation difference or sink, oleic acid two-phase is separated.
In the present invention, the spent acid of the heavy out discharge of the fiber capturing equipment in described step c enters downstream and carries out burning disposal.After method of the present invention processes sulfuric acid alkylation spent acid, hardly containing organic phase in spent acid, by carrying out burning disposal to it, solve spent acid corrodibility large, take equipment many, if the problem that the required investment of other art breading follow-up is larger, and free from environmental pollution, meet environmental requirement.
In a second aspect of the present invention, provide a kind of realize aforesaid method the process of alkylation spent acid and the device that reclaims of organic phase, this device comprises:
For the slurry tank of roughing out, comprise an entrance and a spent acid exports;
For Taylor's emulsion treater of mechanical breakdown of emulsion, comprise a tangential inlet and a lower part outlet; And
For the fiber capturing equipment of oleic acid two-phase laminated flow, comprise an entrance, a light phase export and a heavy out, entrance is connected with the lower part outlet of aforesaid Taylor's emulsion treater.
In the present invention, this device also comprises the alkylation system exported containing entrance and spent acid, containing the impeller pump that a spent acid entrance and a spent acid export, described slurry tank entrance exports with alkylation system spent acid and is connected, described slurry tank spent acid outlet is connected with impeller pump spent acid entrance, the entrance of described Taylor's emulsion treater exports with impeller pump spent acid and is connected, and the described light phase export of fiber capturing equipment is connected with the entrance of alkylation system.
In the prior art, the effect adopting slurry tank gravity settling mode to be separated the organic phase in spent acid is poor, and organic phase acid content is large, and the organic phase obtained also will enter washing process, and water loss is more, increases processing cost.The flow process of other processing method is also all comparatively complicated, and also will consider the further separating-purifying problem of organic phase after reclaiming as added emulsion splitter, secondary pollution problem etc., required equipment and material all increase.Organic phase after recovery is directly returned alkylation system by method of the present invention, realizes the recycle of organic phase, and simultaneously by the oil phase removing in spent acid, meet environmental requirement, technical process is shorter, simple to operate, and equipment is few, invests little.
Below referring to accompanying drawing.
Fig. 1 is alkylation spent acid process according to an embodiment of the invention and organic phase recovery process schema.As shown in Figure 1, raw material and sulfuric acid are sent in alkylation system 1 after carrying out sedimentation rough segmentation process in the spent acid feeding slurry tank 2 produced after carrying out sulfuric acid alkylation reaction, pump in Taylor's emulsion treater 4 through impeller pump 3, to realize the mechanical breakdown of emulsion to spent acid, spent acid after breakdown of emulsion sends into fiber capturing equipment 5, realize oleic acid two-phase laminated flow, the oil phase of gained returns alkylation system 1, and spent acid enters downstream processing.
Fig. 2 A is the diagrammatic cross-section of the Taylor's emulsion treater according to an embodiment of the invention.As shown in Figure 2 A, described Taylor's emulsion treater comprises motor a, entrance b, inner core c, urceolus d, baffle plate e and outlet f, and wherein, urceolus length is L
1, inner core length is L
2, height of baffle plate is H.
Fig. 2 B is the diagrammatic cross-section along the structure of A-A line in Fig. 2 A.As shown in Figure 2 B, outer barrel diameter is D
1, inner diameter of steel flue is D
2, barrier width is B, and baffle length is L
0.
Major advantage of the present invention is:
Method and apparatus equipment of the present invention is simple, and easy to operate, energy loss is few, and processing cost is low; Adopt pure physics mode to carry out the operation such as breakdown of emulsion, separation, do not add chemical reagent, pollution-free; Oleic acid good separating effect, the organic phase rate of recovery is high, economic benefits.
embodiment
The present invention is set forth further below in conjunction with specific embodiment.But, should be understood that these embodiments only do not form limitation of the scope of the invention for illustration of the present invention.The test method of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.Except as otherwise noted, all per-cent and number are by weight.
embodiment 1:
According to method and apparatus of the present invention, alkylation spent acid is carried out to the reclaimer operation of the process such as rough segmentation, breakdown of emulsion, separation and organic phase.
The method comprises: pump into Taylor's emulsion treater after the spent acid that sulfuric acid alkylation produces is carried out sedimentation rough segmentation process in slurry tank, realize the mechanical breakdown of emulsion to spent acid, spent acid after breakdown of emulsion passes into fiber capturing equipment, realize oleic acid two-phase laminated flow, oil phase returns alkylation system, and spent acid enters downstream processing.
This device comprises: alkylation system, slurry tank, impeller pump, Taylor's emulsion treater and fiber capturing equipment; The spent acid outlet of alkylation system is connected with slurry tank; The spent acid outlet of slurry tank is connected with impeller pump; The outlet of impeller pump spent acid is connected with Taylor's emulsion treater; The lower part outlet of Taylor's emulsion treater is connected with fiber capturing equipment; The light phase export of fiber capturing equipment is connected to alkylation system.
Processing condition:
Acid-spending strength is 85%, and organic phase content is 15%, and in gravity settler, the settling time is 2 hours; Taylor's emulsion treater urceolus length L
1, inner core length L
2, outer barrel diameter D
1, inner diameter of steel flue D
2, L
1=1D
1, D
2=0.5D
1, L
2=0.5L
1; Outer tube inner wall is provided with 2 layers of baffle plate, barrier width B, length L
0, be highly H, H=2L
0, L
0=2B, every layer of baffle plate arranged is 4, and entrance flow velocity is 20m/s; Totally two sections, fiber capturing layer in fiber capturing equipment, first paragraph fiber capturing layer material is tetrafluoroethylene, and second segment fiber capturing layer material is 304 stainless steels.
Experimental result:
After treatment, the organic phase acid content of fiber capturing equipment light phase export is 71ppm to spent acid, and the spent acid oleaginousness of fiber capturing equipment heavy out is less than 1% (V/V).
embodiment 2:
According to the method and apparatus identical with embodiment 1, alkylation spent acid is carried out to rough segmentation, breakdown of emulsion, the reclaimer operation of process and organic phase such as to be separated.
Processing condition:
Acid-spending strength is 83%, and organic phase content is 17%, and in gravity settler, the settling time is 2 hours, and acid-spending strength is 85%, and organic phase content is 15%, and in gravity settler, the settling time is 2 hours; Taylor's emulsion treater urceolus length L
1, inner core length L
2, outer barrel diameter D
1, inner diameter of steel flue D
2, L
1=2D
1, D
2=0.6D
1, L
2=0.6L
1; Outer tube inner wall establishes the baffle plate that haves three layers, barrier width B, length L
0, be highly H, H=2L
0, L
0=2B, every layer of baffle plate arranged is 8, entrance flow velocity 20m/s; Totally two sections, fiber capturing layer in fiber capturing equipment, first paragraph fiber capturing layer material is polypropylene, and second segment fiber capturing layer material is 304 stainless steels.
Experimental result:
After treatment, the organic phase acid content of fiber capturing equipment light phase export is 61ppm to spent acid, and the spent acid oleaginousness of fiber capturing equipment heavy out is less than 1% (V/V).
embodiment 3:
According to the method and apparatus identical with embodiment 1, alkylation spent acid is carried out to rough segmentation, breakdown of emulsion, the reclaimer operation of process and organic phase such as to be separated.
Processing condition:
Acid-spending strength is 85%, and organic phase content is 15%, and in gravity settler, the settling time is 2 hours, and Taylor's emulsion treater acid-spending strength is 85%, and organic phase content is 15%, and in gravity settler, the settling time is 2 hours; Taylor's emulsion treater urceolus length L, urceolus length L
1, inner core length L
2, outer barrel diameter D
1, inner diameter of steel flue D
2, L
1=3D
1, D
2=0.8D
1, L
2=0.8L
1; Outer tube inner wall establishes the baffle plate that is of five storeys, barrier width B, length L
0, be highly H, H=2L
0, L
0=2B, every layer of baffle plate arranged is 16, entrance flow velocity 20m/s; Totally two sections, fiber capturing layer in fiber capturing equipment, first paragraph fiber capturing layer material is tetrafluoroethylene, and second segment fiber capturing layer material is modification steel wire.
Experimental result:
After treatment, the organic phase acid content of fiber capturing equipment light phase export is 45ppm to spent acid, and the spent acid oleaginousness of fiber capturing equipment heavy out is less than 1% (V/V).
Above-mentioned listed embodiment is only preferred embodiment of the present invention, is not used for limiting practical range of the present invention.Namely all equivalences done according to the content of the present patent application the scope of the claims change and modify, and all should be technology category of the present invention.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read above-mentioned teachings of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (10)
1. a method for the process of alkylation spent acid and organic phase recovery, the method comprises the following steps:
A. the spent acid that sulfuric acid alkylation produces is carried out sedimentation rough segmentation process;
B. the spent acid through sedimentation rough segmentation process is carried out mechanical breakdown of emulsion process;
C. the spent acid after mechanical breakdown of emulsion process is carried out oleic acid two-phase laminated flow, the oil phase of gained returns alkylation system, and the spent acid of gained enters downstream processing.
2. the method for claim 1, is characterized in that, in described step a, use gravity settling or silk screen foam removal to carry out sedimentation rough segmentation process, the settling time is 0-2 hour.
3. the method for claim 1, is characterized in that, in described step a, the acid concentration of described spent acid is lower than 91%, and the organic phase content in spent acid is 10-30%.
4. the method for claim 1, is characterized in that, in described step c, the spent acid of gained enters downstream and carries out burning disposal.
5. a device for the process of alkylation spent acid and organic phase recovery, this device comprises:
Spent acid for being produced by sulfuric acid alkylation carries out the slurry tank (2) of sedimentation rough segmentation process, and it comprises an entrance and spent acid outlet;
Be connected with slurry tank (2), for the spent acid through sedimentation rough segmentation process being carried out Taylor's emulsion treater (4) of mechanical breakdown of emulsion process, it comprises a tangential inlet and a lower part outlet; And
Be connected with Taylor's emulsion treater (4), for the spent acid after mechanical breakdown of emulsion process being carried out the fiber capturing equipment (5) of oleic acid two-phase laminated flow, it comprises an entrance, a light phase export and a heavy out, and this entrance is connected with the lower part outlet of Taylor's emulsion treater (4).
6. device as claimed in claim 5, it is characterized in that, this device also comprises: alkylation system (1), and it comprises entrance and spent acid outlet; And impeller pump (3), it comprises a spent acid entrance and spent acid outlet, wherein, the entrance of described slurry tank (2) exports with the spent acid of alkylation system (1) and is connected, the spent acid outlet of described slurry tank (2) is connected with the spent acid entrance of impeller pump (3), the tangential inlet of described Taylor's emulsion treater (4) exports with the spent acid of impeller pump (3) and is connected, and the light phase export of described fiber capturing equipment (5) is connected with the entrance of alkylation system (1).
7. the device as described in claim 5 or 6, is characterized in that, described Taylor's emulsion treater (4) is double-barrel structure, and spent acid enters urceolus through tangential inlet, and urceolus is static, and motor drives inner cylinder rotating; Urceolus length is L
1, inner core length is L
2, outer barrel diameter is D
1, inner diameter of steel flue is D
2, wherein L
1=1D
1~ 3D
1, D
2=0.5D
1~ 0.9D
1, L
2=0.5L
1~ 0.8L
1; Outer tube inner wall is provided with 0-5 layer baffle plate, and barrier width is B, and length is L
0, be highly H, wherein H=1L
0~ 5L
0, L
0=1B ~ 3B; The baffle plate that outer tube inner wall every layer is arranged is 0-16, and outer tube inner wall distributes symmetrically and evenly.
8. device as claimed in claim 7, it is characterized in that, the pressure of described Taylor's emulsion treater (4) reduces to 0-50KPa, and entrance flow velocity is 1-30m/s; When inner core high speed rotating, spent acid can form Taylor vortex flow between inner/outer tube, utilizes the shearing force between drop and impact force to realize breakdown of emulsion, makes organic phase agglomeration.
9. the device as described in claim 5 or 6, is characterized in that, described fiber capturing equipment (5) is made up of shell and fiber capturing layer, and wherein, fiber capturing layer is woven by fine-fibered and forms, and the diameter of fiber is 10-200um.
10. device as claimed in claim 9, it is characterized in that, the material of described fiber capturing layer is organic materials or metallic substance, and organic materials and metallic substance can be used alone or mixed weaving uses; Described fine-fibered has hydrophilic or lipophilicity, and when oleic acid two-phase is passed through, oleophylic fine-fibered catches thin organic phase, makes organic phase agglomeration become larger oil droplet, accelerates oleic acid two-phase laminated flow.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610120430.6A CN105540900B (en) | 2016-03-03 | 2016-03-03 | The method and apparatus for being alkylated waste acid treatment and organic phase recycling |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610120430.6A CN105540900B (en) | 2016-03-03 | 2016-03-03 | The method and apparatus for being alkylated waste acid treatment and organic phase recycling |
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| 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 |
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| CN105540900B (en) | 2018-11-20 |
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