CN106975430B - A kind of two-phase mixtures reactor and its application - Google Patents
A kind of two-phase mixtures reactor and its application Download PDFInfo
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- CN106975430B CN106975430B CN201610028079.8A CN201610028079A CN106975430B CN 106975430 B CN106975430 B CN 106975430B CN 201610028079 A CN201610028079 A CN 201610028079A CN 106975430 B CN106975430 B CN 106975430B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G19/00—Refining hydrocarbon oils in the absence of hydrogen, by alkaline treatment
- C10G19/02—Refining hydrocarbon oils in the absence of hydrogen, by alkaline treatment with aqueous alkaline solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/248—Reactors comprising multiple separated flow channels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/24—Stationary reactors without moving elements inside
- B01J2219/2401—Reactors comprising multiple separate flow channels
Abstract
The present invention relates to refining arts, disclose a kind of two-phase mixtures reactor and its application, the two-phase mixtures reactor includes reactor inlet, reactor outlet, reactor tank body and reaction module, the outer surface of reaction module is provided with groove structure, the protrusion side wall of groove structure is connect with reactor tank body, it is formed by groove structure with the cavity that reactor tank body surrounds and mixes runner, cavity unit is arranged in the inside of reaction module, cavity unit passes through the distribution hole that the bottom of groove structure of reaction module is arranged in and is connected to runner is mixed, the setting of the entrance of cavity unit is so that flow direction of the fluid in cavity unit is opposite with the flow direction in mixing runner.Two-phase mixtures reactor of the invention is in the deep desulfuration for lighter hydrocarbons, so that lighter hydrocarbons and lye flow at high speed and being vigorously mixed, resistance to mass tranfer is low, realizes deep desulfuration, acid sulphur-containing substance removal efficiency is greater than 90%, and acid sulphur-containing substance concentration can be down to 10ppm or less or lower in liquefied gas.
Description
Technical field
The present invention relates to refining arts, and in particular, to a kind of two-phase mixtures reactor and the two-phase mixtures reactor
Application in liquid liquid two-phase or gas/liquid two-phase mixtures and reaction.
Background technique
Containing a large amount of acid sulphur-containing substances (predominantly hydrogen sulfide and mercaptan) in the thick liquefied gas that oil plant generates, industrially
The general method by alkali cleaning removes acid sulphur-containing substance therein.
(acid sulphur-containing substance concentration can be used for producing cleaning combustion in 10ppm or less) to liquefied gas after deep desulfuration
Material.But conventional desulfuration of liquefied gas equipment is difficult to overcome in deep desulfurization process in the case where operating condition is basically unchanged
Resistance to mass tranfer, it is therefore desirable to develop efficient liquefied gas deep desulfuration reactor, realize the liquid under low mass transfer Impetus Condition
Change the requirement of gas deep desulfuration.
It is used since the technology that the method by alkali cleaning carries out desulfuration of liquefied gas is related to liquid liquid two-phase system
Equipment generally comprises several classes such as extraction tower, static mixer and fiber film abstractor.
Extraction tower be a kind of continuous flow upstream equipment, it can be achieved that multiple theoretical stages separative efficiency, but its equipment scale compared with
Greatly, operation is more complicated, and material flow is slower, and mass tranfer coefficient is lower.
Fiber film abstractor is a kind of cocurrent cooling operation equipment, and equipment scale is small compared with extraction tower, and uses hydrophilic fibre
Silk provides biggish mass transfer area, therefore mass-transfer efficiency is higher, but fiber filament can be contaminated and lose after being used for a long time
Hydrophily, mass-transfer efficiency reduce, and are difficult to cleaning regeneration.
The equipment scale of static mixer is minimum, mixes by two-phase flow at high speed and carries out mass transport process, but static mixed
The mixed structure of clutch is difficult to realize the high degree of dispersion mixing of liquid liquid system, therefore there is also larger for the raising of its mass-transfer efficiency
Bottleneck.
Summary of the invention
The purpose of the present invention is overcoming the deficiencies of existing technologies, it is suitable under low mass transfer Impetus Condition to provide a kind of satisfaction
For liquid liquid two-phase or gas/liquid two-phase mixtures and the two-phase mixtures reactor of reaction.
To achieve the goals above, in a first aspect, the present invention provides a kind of two-phase mixtures reactor, two-phase mixtures reaction
Device includes reactor inlet, reactor outlet, reactor tank body and reaction module, the outer surface of the reaction module be provided with to
Few two groove structures, the protrusion side wall of the groove structure are connect with the inner wall of the reactor tank body, the groove structure
It is formed between the inner wall of the reactor tank body and mixes runner, the reaction module is internally provided with cavity unit, described
Cavity unit is connected to by the way that the distribution hole of the bottom of the groove structure of the reaction module is arranged in the mixing runner,
In, the setting of the entrance of the cavity unit is so that flow direction of the fluid in the cavity unit mixes runner with described
In flow direction it is opposite；It is described mixing runner entrance and it is described mixing runner outlet respectively with the reactor inlet and
The reactor outlet keeps connection.
Second aspect, the present invention provide aforementioned two-phase mixtures reactor in liquid liquid two-phase or gas/liquid two-phase mixtures and reaction
In application.
Two-phase mixtures reactor provided by the invention be used for lighter hydrocarbons, such as liquefied gas deep desulfuration when, enable to
Lighter hydrocarbons and lye flow at high speed and are vigorously mixed in two-phase mixtures reactor of the invention, and resistance to mass tranfer is low, so that liquefied gas
In contained acid sulphur-containing substance (such as mercaptan) sufficiently reacted with lye, realize that liquefied gas deep desulfuration, acid sulphur-containing substance take off
Except rate is greater than 90%, acid sulphur-containing substance concentration can be down to 10ppm or less or lower in liquefied gas.
Two-phase mixtures reactor provided by the invention is particularly suitable for sulfur-bearing acid in lighter hydrocarbons, such as liquefied gas or light petrol
Material concentration is lower (such as tens ppm), thus carries out deep desulfuration in the lower situation of mass transfer force.At this point, reaction
Two-phase mixed at high speed contacts in device, and resistance to mass tranfer is very low, and the acidity sulphur-containing substance such as mercaptan can contacted fully instead with lye
The separation of Ying Houyu lighter hydrocarbons.
Two-phase mixtures reactor provided by the invention also has reactor for treatment amount big, and structure is simple, and size is small, resistance to pressure energy
Power is strong, and is convenient for the advantages of sealing, install and safeguarding.
Two-phase mixtures reactor provided by the invention, before two-phase mixtures contact, flowing side of the two-phase in respective runner
To preferably countercurrent flow, reflux type can make the pressure difference of each distribution hole two sides be uniformly distributed, and a phase can be equably
From each distribution hole flow out and with another mixing that is in contact, thus in two-phase mixtures reactor realization multistage cross flow be mixed
Effect, strengthen mass-transfer performance, avoiding the part distribution hole as caused by Pressure difference distribution is uneven can not push fluid out, thus
The phenomenon that reducing mass-transfer efficiency.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the cross-sectional structure schematic diagram of the two-phase mixtures reactor of a preferred embodiment of the invention.
Fig. 2 is the vertical section structure schematic diagram of the two-phase mixtures reactor of a preferred embodiment of the invention.
Fig. 3 is the flow chart of the method for the lighter hydrocarbons deep desulfuration of a preferred embodiment of the invention.
Description of symbols
1, reactor inlet 2, reactor outlet
3, reactor tank body 4, reaction module
5, cavity unit 6, mixing runner
7, dispersed phase introduces pipe 8, distribution hole
9, protrusion side wall 10, distributing chamber
11, collecting chamber 12, caustic wash unit
13, sedimentation unit 14, oxidation regeneration unit
15, anti-extraction unit 16, fresh lye
17, sulfur-bearing lighter hydrocarbons 18, regeneration lye
19, sulfur-bearing lye 20, oxygen-containing gas
21, light-end products 22, sulfur-bearing light-end products
23, desulfurization lighter hydrocarbons
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
In a first aspect, the two-phase mixtures reactor includes that reactor enters the present invention provides a kind of two-phase mixtures reactor
Mouth, reactor outlet, reactor tank body and reaction module, the outer surface of the reaction module are provided at least two groove knots
Structure, the protrusion side wall of the groove structure are connect with the inner wall of the reactor tank body, the groove structure and the reactor
Mixing runner is formed between the inner wall of tank body, the reaction module is internally provided with cavity unit, and the cavity unit passes through
The distribution hole that the bottom of the groove structure of the reaction module is arranged in is connected to the mixing runner, wherein the cavity list
Member entrance setting so that flow direction of the fluid in the cavity unit in the flow direction mixed in runner
On the contrary；The outlet of the entrance of the mixing runner and the mixing runner goes out with the reactor inlet and the reactor respectively
Mouth keeps connection.
In the present invention, the protrusion side wall of the groove structure is connect with the inner wall of the reactor tank body, so that being formed
Each mixing runner keep mutually indepedent, in the contact and reaction process of fluid, the fluid between each item mixing runner is not
It can interfere with each other.
The outer shape of the two-phase mixtures reactor is not required particularly, can for cylindrical shape, rectangular-shape,
Elliptic Cylinder shape, cube-shaped, prism-shaped etc., under preferable case, the two-phase mixtures reactor is cylindrical shape.
Preferably, the two-phase mixtures reactor further comprises collecting chamber and distributing chamber, and the reactor inlet is through institute
The entrance that distributing chamber is connected to the mixing runner is stated, the outlet of the mixing runner is connected to the reactor through the collecting chamber and goes out
Mouthful.Distributed component can be contained in the distributing chamber of the invention.
Preferably, the space that the inner wall of reactor tank body surrounds is cylindrical shape, Elliptic Cylinder shape, cube-shaped and rectangular
At least one of body shape；The space that the inner wall of the more preferable reactor tank body surrounds is cylindrical shape.
Preferably, the bottom of the cavity unit is provided with so that the fluid enters the dispersion coupling of the cavity unit
Enter pipe.
Preferably, the number of the distribution hole of the bottom of each groove structure is identical or different, and each groove
The number of the distribution hole of the bottom of structure is each independently 1-100.
Preferably, the aperture of each distribution hole is 0.1-2mm.
Preferably, according to the flow direction of the fluid in the cavity unit, the aperture of the distribution hole is sequentially increased.
Preferably, according to the flow direction of the fluid in the cavity unit, the aperture ratio downstream phase of the distribution hole of upstream
The small 0.01-1mm in aperture of adjacent distribution hole.
Preferably, in the bottom of each groove structure, the distance of the central point of two neighboring distribution hole is 0.5-
40mm；More preferably 1-30mm.
Preferably, the depth of the distribution hole is 0.1-3mm；More preferably 0.3-2.5mm.
Preferably, the axial direction of the distribution hole is any angle with the angle of the flow direction of the fluid mixed in runner,
It is preferred that the angle is 45-90 degree, more preferably 90 degree.
Preferably, the distribution hole is point-blank successively set along the fluid flow direction in the mixing runner
It sets.But the setting of the distribution hole is not limited thereto, and when the number of the distribution hole is more than one, the distribution
Hole can not also be configured along the straight line parallel with the fluid flow direction in mixing runner.
The distribution hole can be set in the entire bottom of each groove structure, it is preferable that the distribution hole setting
In proximal response device arrival end, to be conducive to the fluid from the cavity unit and the fluid energy from the reactor inlet
It reaches the nearly entrance end in contact in the mixing runner and reacts, and the fluid-mixing obtained after mixing can be mentioned in reaction module
Make contact and the reaction of fluid-mixing more abundant in the longer mixing runner supplied.Preferably, it is provided with the close anti-of distribution hole
Answer the internal diameter of the cavity unit of device arrival end identical and center line having the same.
Preferably, according to the flow direction of the fluid in the cavity unit, the entrance of the cavity unit is arranged in institute
The upstream of cavity unit is stated, also, the upstream of each distribution hole is arranged in the entrance of the cavity unit.
Preferably, at least one fiber filament can be set in the mixing runner.The filametntary material can be gold
The inorganic material such as category, glass are also possible to organic material, or the composite material of the above different materials.Filametntary selection root
Depending on property according to the fluid in cavity unit, if the fluid in cavity unit is aqueous solution, fiber filament is optional
With hydrophilic materials such as stainless steel or glass；If the fluid in cavity unit is oil product, oleophylic is can be selected in fiber filament
The organic material of property.It is preferred that the filametntary diameter is 1 μm to 5mm, more preferably 2-50 μm.Fiber is added in mixing runner
Silk, can be formed by the compatibility of drop with the fluid in cavity unit by it, be formed in filament surface very thin
Liquid film, increase interphase mass transfer area, shorten mass transfer distance, improve mixing efficiency.
To the filametntary diameter and length, there is no particular limitation, and those skilled in the art can be according in the art
Conventional parameter selected.The filametntary length can be arranged, the fiber according to the length of the mixing runner
Silk can mix runner through entire, and preferably according to the fluid flow direction in mixing runner, the filametntary length is
From the central point of the distribution hole of most downstream to the distance of mixing runner exit.
Under preferable case, the fiber filament is linear or helical form.
Preferably, the open at one end of the cavity unit is fluid inlet, and the other end is closed end.That is, fluid
Cavity unit can be entered by fluid inlet, and entered by the distribution hole of connection cavity unit and the mixing runner
It is contacted and/or is reacted with the fluid from the reactor inlet in the mixing runner in mixing runner, and from
The outlet of the mixing runner leads to the reactor outlet.
Preferably, the connection type between the protrusion side wall of the groove structure and the inner wall of the reactor tank body includes
Detachable connection method and non-detachable connection method.
Preferably, the connection type between the protrusion side wall of the groove structure and the inner wall of the reactor tank body is selected from
Welded connecting threaded connection, expanded joint, stings seam connection, is glued and at least one of connects with blind rivet.
Preferably, the reaction module includes that multiple groove structures are conducive to make to form multiple mixing runners
Obtaining two-phase mixtures reactor of the present invention has biggish processing capacity, it is preferable that the distance between adjacent mixing runner
For 0.5mm-10mm, the distance between the adjacent mixing runner at this is the thickness of the protrusion side wall between adjacent mixing runner
Degree.
Preferably, the cross-sectional area in each mixing runner perpendicular to fluid flow direction is 0.5-20mm2, preferably
For 1-10mm2。
According to a kind of preferred embodiment, the cross-sectional structure of the two-phase mixtures reactor of the invention is illustrated
For figure as shown in Figure 1, specifically, the two-phase mixtures reactor includes that reactor inlet (not shown), reactor outlet (do not show
Out), reactor tank body 3 and reaction module 4, the outer surface of the reaction module 4 is provided at least two, and (example is arranged as shown in figure 1
Have 11) groove structure, the protrusion side wall 9 of the groove structure connect with the inner wall of the reactor tank body 3, the groove knot
The inner wall formation of structure and the reactor tank body 3 mixes runner 6, the reaction module 4 be internally provided with cavity unit 5 and
So that the dispersed phase that fluid enters the cavity unit 5 introduces pipe 7, the cavity unit 5 is by being arranged in the reaction module 4
The distribution hole 8 of bottom of groove structure be connected to the mixing runner 6, the setting of the entrance of the cavity unit 5 is so that stream
Body is opposite with the flow direction in the mixing runner 6 in the flow direction in the cavity unit 5；The mixing runner 6
Entrance and it is described mixing runner 6 outlet respectively with the reactor inlet and the reactor outlet holding be connected to.At this
In the preferred embodiment of invention, the reactor tank body and reaction module are disposed as cylindrical, however, of the invention
The two-phase mixtures reactor may be set to be the shapes such as triangular prism, quadrangular, and those skilled in the art should not will be above-mentioned excellent
The cylindrical shape of choosing is interpreted as limitation of the present invention.
According to another preferred embodiment, the vertical section structure of the two-phase mixtures reactor of the invention shows
It is intended to as shown in Fig. 2, specifically, the two-phase mixtures reactor includes reactor inlet 1, reactor outlet 2, reactor tank body
3 and reaction module 4, the outer surface of the reaction module be provided at least two groove structures, the raised sides of the groove structure
Wall is connect with the inner wall of the reactor tank body, and the groove structure mixes runner 6 with the formation of the inner wall of the reactor tank body,
The reaction module is internally provided with cavity unit 5, and the cavity unit 5 passes through the groove that the reaction module 4 is arranged in
The distribution hole 8 of the bottom of structure is connected to the mixing runner 6, the setting of the entrance of the cavity unit 5 so that fluid in institute
The flow direction stated in cavity unit 5 is opposite with the flow direction in the mixing runner 6；The entrance of the mixing runner 6
It is connected to respectively with the reactor inlet 1 and the holding of the reactor outlet 2 with the outlet of the mixing runner 6；First fluid
Entered in the two-phase mixtures reactor by the reactor inlet 1, successively by the entrance of distributing chamber 10 and mixing runner 6
Into in the mixing runner 6, and in the mixing runner 6 and successively by the dispersed phase inlet tube 7, cavity unit 5
It is mixed with the second fluid of the distribution hole 8, gained mixture enters collecting chamber 11 through the outlet of the mixing runner 6
In and the outlet of reacted device 2 lead to except the two-phase mixtures reactor.
Second aspect, the present invention provide aforementioned two-phase mixtures reactor in liquid liquid two-phase or gas/liquid two-phase mixtures and reaction
In application.Hybrid reaction process including water phase with oily phase, the hybrid extraction process of water phase and oily phase, gas phase and liquid phase are mixed
Reaction process etc. is closed, specifically, such as can be used for solvent deasphalting process or aqueous solution absorption H2The soluble gas such as S
Process.
Under preferable case, two-phase mixtures reactor provided by the invention is used for lighter hydrocarbons deep desulfurization process.The lighter hydrocarbons
For the petroleum hydrocarbon-fraction of the C4-C5 containing acid sulphur-containing substance, wherein the acid sulphur-containing substance is mercaptan, in terms of element sulphur
Sulfur content in the lighter hydrocarbons is 50-2000ppm.
The third aspect, the present invention provide a kind of method of lighter hydrocarbons deep desulfuration, and this method is including caustic wash unit, sedimentation list
Implement in the system of member, oxidation regeneration unit and anti-extraction unit, lighter hydrocarbons pass through caustic wash unit and the contained acid of sedimentation unit removal
Property sulphur-containing substance, and lye realizes regeneration by oxidation regeneration unit and anti-extraction unit.
In the present invention, the caustic wash unit includes present invention two-phase mixtures reactor above-mentioned.
In the method for lighter hydrocarbons deep desulfuration of the present invention, in lye and lighter hydrocarbons, (lighter hydrocarbons are before treatment
Sulfur-bearing, therefore hereinafter also referred to sulfur-bearing lighter hydrocarbons, be desulfurization lighter hydrocarbons in the lighter hydrocarbons obtained after desulfurization) liquid liquid that is formed
In two phase flow, a phase is as continuous phase, and another phase is as dispersed phase.
The step of caustic wash unit in the method for lighter hydrocarbons deep desulfuration of the invention includes: entering from cavity unit by lye
Mouth is introduced into cavity unit, and the lye is entered mixed with the lighter hydrocarbons mixed in runner in mixing runner by the distribution hole
Close reaction, wherein flow direction of the lye in cavity unit is mixing the flow direction phase in runner with the lighter hydrocarbons
Instead.
In the method for lighter hydrocarbons deep desulfuration of the present invention, NaOH can be contained in the lye, preferably NaOH's
Concentration is 10-20 weight %.In the caustic wash unit, the acid sulphur-containing substance in sulfur-bearing lighter hydrocarbons is reacted with NaOH generates sulfur-bearing
Sodium salt, and sulfur-bearing sodium salt is dissolved in lye.Enter alkali cleaning list by the mixture that the lighter hydrocarbons and lye of desulphurization reaction are formed
After carrying out initial gross separation in the precipitation apparatus of member, the lighter hydrocarbons after just dividing then are introduced into sedimentation unit, the lye that will wherein carry secretly
After being sufficiently separated, desulfurization lighter hydrocarbons are obtained, the desulfurization lighter hydrocarbons, which can enter the processes such as subsequent washing purification, to be continued
Processing.
In the method for lighter hydrocarbons deep desulfuration of the present invention, the sulfur-bearing lye and sedimentation unit that are discharged by caustic wash unit
Discharge sulfur-bearing lye mixing after enter oxidation regeneration unit in, with oxygen-containing gas (typically air, oxygen rich gas or
Oxygen) it is contacted.The reactor of oxidation regeneration unit typically bubbling bed reactor and/or the reaction of filler bubbling bed
Device.In the reactor of oxidation regeneration unit, sulfur-bearing sodium salt and oxygen-containing gas in sulfur-bearing lye (contain sulfonation phthalein in catalyst
The ARI 100EXL catalyst of cyanines cobalt or other substances with catalytic action) under the action of react, by containing in sulfur-bearing lye
Sulphur sodium salt is converted into disulphide not soluble in water, the lye after obtaining desulfurization.
In the method for lighter hydrocarbons deep desulfuration of the present invention, disulphide does not dissolve in lye, therefore again by oxidation
The precipitation apparatus in unit is given birth to separate the lye after disulphide and desulfurization.Since the density of lye and disulphide connects very much
Closely, it still containing a large amount of disulphide in the lye after the desulfurization being discharged by oxidation regeneration unit, needs to enter anti-extraction unit
The separation of lye and disulphide after continuing desulfurization.Under preferable case, institute of the present invention is used in the anti-extraction unit
The two-phase mixtures reactor stated.
In the method for lighter hydrocarbons deep desulfuration of the present invention, for the two-phase mixtures reactor of caustic wash unit, preferably
Sulfur-bearing lighter hydrocarbons are as continuous phase, and lye is as dispersed phase；And for the two-phase mixtures reactor of anti-extraction unit, preferably lye is
Continuous phase, petroleum benzin are dispersed phase.In anti-extraction unit of the invention, the petroleum benzin as dispersed phase can be this field
Interior conventional use of various gasoline.
In the method for lighter hydrocarbons deep desulfuration of the present invention, in the anti-extraction unit, by the lye after desulfurization
It is soluble in light-end products therein such as gasoline in the two-phase mixtures reactor with disulphide to contact, after realizing desulfurization
The separation of lye and the disulphide wherein carried secretly obtains regeneration lye.Precipitation apparatus through anti-extraction unit, regeneration lye with
Light-end products separation containing disulphide, is recycled back to the caustic wash unit for the regeneration lye and carries out lighter hydrocarbons desulfurization.Described
It is similar to the operating method of caustic wash unit using the operating method of two-phase mixtures reactor of the present invention in anti-extraction unit,
Details are not described herein by the present invention.
In the method for lighter hydrocarbons deep desulfuration of the present invention, the reaction condition of the preferably described caustic wash unit includes: anti-
Answering temperature is 25-80 DEG C, reaction pressure 0.2-2MPa.
The method of lighter hydrocarbons deep desulfuration according to the present invention, preferably dispersed phase introduce the inlet of pipe in dispersed phase
Apparent velocity is 0.2-5m/s, more preferably 0.3-3m/s.
In the method for lighter hydrocarbons deep desulfuration of the present invention, the reaction condition of the preferably described anti-extraction unit includes:
Reaction temperature is 25-80 DEG C, reaction pressure 0.2-2MPa.
The apparent stream of the method for lighter hydrocarbons deep desulfuration according to the present invention, preferably continuous phase in mixing flow passage entry
Speed is 0.5-20m/s, more preferably 4-10m/s.
In the method for lighter hydrocarbons deep desulfuration of the present invention, swiftly flowing liquid liquid two in two-phase mixtures reactor
It is mutually vigorously mixed, the drop and continuously mix acutely that dispersed phase is formed, resistance to mass tranfer is low, enables to the mass transfer between two-phase
Process sufficiently carries out, and desulfuration efficiency can reach 90% or more, that is to say, that can make contained acid in lighter hydrocarbons in caustic wash unit
Property sulphur-containing substance (such as mercaptan) is sufficiently reacted with lye, realizes that the deep desulfuration of lighter hydrocarbons, acid sulphur-containing substance removal efficiency are greater than
90 weight %, the mass concentration of acid sulphur-containing substance can be down to 10ppm or less in lighter hydrocarbons；And alkali may be implemented in anti-extraction unit
Being sufficiently mixed for liquid and light-end products, is extracted to oily phase (light-end products) for the disulphide of entrained in the lye after desulfurization
In, the extraction yield of disulphide is greater than 90 weight %.
In the method for lighter hydrocarbons deep desulfuration of the present invention, the pressure drop preferably in two-phase mixtures reactor is 10-
800kPa；More preferably 100-600kPa.Dispersed phase forms drop after distribution hole and is mixed with continuous phase.Due to distribution
The diameter in hole is smaller, therefore the size of drop is also smaller, can obtain biggish interphase mass transfer area.
Two-phase mixtures reactor provided by the invention can be to two since the movement velocity of dispersed phase and continuous phase is very high
The runner for mixing reactor is adequately washed away, and the problem of runner blocks during long-term operation is avoided.It considers
This higher feature of the interfacial tension of liquid liquid system, method of the invention realize that lighter hydrocarbons depth is de- by being vigorously mixed for two-phase
The purpose of sulphur in liquid liquid two-phase contact process and does not use any substance (such as surface-active with reduction system tension
Agent, alcohols etc.) promote two-phase mixtures to contact, therefore avoid the emulsion of system, split-phase is imitated after two-phase mixtures contact
Fruit is good, and not additional waste material generates.
By anti-extraction unit be discharged regeneration lye in sulfur content it is lower, can hardly using other extraction steps into
One step reduces sulfur content, therefore returning to sulphur contained in the regeneration lye of caustic wash unit substantially will not be by lighter hydrocarbons in alkaline cleaning procedure
It extracts and the desulfurization degree in lighter hydrocarbons is impacted.
According to the treating capacity of the concentration of the acid sulphur-containing substance in lighter hydrocarbons and lighter hydrocarbons, two-phase provided by the invention can be mixed
It closes reactor and carries out separate unit or multi-platform combined use.
Preferred embodiment according to the present invention, two-phase mixtures reactor provided by the invention is using more series connection
Form uses, and the reaction condition in each two-phase mixtures reactor can be identical or different, each independently includes: reaction
Temperature is 25-80 DEG C, reaction pressure 0.2-2MPa.
The method of a kind of preferred embodiment according to the present invention, lighter hydrocarbons deep desulfuration of the present invention uses
Technique in flow chart shown in Fig. 3 carries out, specifically:
In the method for lighter hydrocarbons deep desulfuration of the present invention, by fresh lye 16 and/or regeneration lye 18 and sulfur-bearing
Lighter hydrocarbons 17 are introduced into caustic wash unit 12, in the caustic wash unit 12, in the acid sulphur-containing substance and lye in sulfur-bearing lighter hydrocarbons
NaOH reaction generates sulfur-bearing sodium salt, and sulfur-bearing sodium salt is dissolved in lye.Just divided by the lighter hydrocarbons and lye of caustic wash unit
Enter in sedimentation unit 13 afterwards, the lighter hydrocarbons after just dividing obtain desulfurization lighter hydrocarbons after being sufficiently separated in the sedimentation unit
23, desulfurization lighter hydrocarbons 23 enter the processes such as subsequent washing purification and are continued with.By sedimentation unit discharge lye with come from
The lye of caustic wash unit is formed together sulfur-bearing lye 19 and enters in oxidation regeneration unit 14, is contacted with oxygen-containing gas 20.?
In the reactor of oxidation regeneration unit, the sulfur-bearing sodium salt in sulfur-bearing lye is reacted with oxygen-containing gas 20, by containing in sulfur-bearing lye
Sulphur sodium salt is converted into disulphide, the lye after obtaining desulfurization.Lye after the desulfurization be discharged by oxidation regeneration unit enters anti-
Extraction unit 15 continues the separation of lye and disulphide after desulfurization.In the anti-extraction unit 15, after desulfurization
Lye is contacted with light-end products 21, the separation of the lye after realizing desulfurization and the disulphide wherein carried secretly, obtains regeneration lye
18 and sulfur-bearing light-end products 22.The regeneration lye 18 is recycled back to progress lighter hydrocarbons desulfurization in the caustic wash unit 12.
Two-phase mixtures reactor provided by the invention and its application also have the advantages that following specific:
Two-phase mixtures reactor is coupled in lighter hydrocarbons sulfur removal technology, the special construction design of two-phase mixtures reactor both may be used
To strengthen above-mentioned reaction process, and can be with idetified separation process.Two-phase mixtures reactor uses special mixing runner design,
Liquid liquid two-phase mixed at high speed in two-phase mixtures reactor, enhances mass transport process, realizes lighter hydrocarbons deep desulfuration, can will be light
Acid sulphur-containing substance concentration in hydrocarbon is down to the even lower level of 10ppm, and desulfurization degree is up to 90 weight % or more.Two-phase mixtures are anti-
The problem of answering two-phase apparent velocity height in device, being not susceptible to runner blocking.Utilize the high feature of interface tension, it is not necessary to use
Surface reactive material avoids emulsification problem in two-phase mixtures reactor, after two-phase mixtures contact, convenient for split-phase and carries out subsequent
Processing.The treating capacity of two-phase mixtures reactor is big, and structure is simple, and size is small, and voltage endurance capability is strong, and convenient for sealing, installation and dimension
Shield.
The present invention will be described in detail by way of examples below.
Below in case of no particular description, used a variety of materials are all from commercially available.
Embodiment 1
The present embodiment carries out lighter hydrocarbons desulfurization using two-phase mixtures reactor of the present invention, specifically as follows:
Liquefied gas and lye containing mercaptan contact in caustic wash unit, and mercaptan is reacted with the NaOH in lye generates mercaptan
Sodium is simultaneously dissolved in lye.It is completed after being entered sedimentation unit by the liquefied gas that caustic wash unit is discharged and separated with the part lye that it is carried secretly
The purpose of removal of mercaptans.By sedimentation unit be discharged lye enter oxidation regeneration unit, in filler bubbling bed reactor, lye with
Sodium mercaptides are converted disulphide by air haptoreaction.Lye after the desulfurization being discharged by oxidation regeneration unit enters back suction
Bill of lading member, contacts with gasoline, removes the disulphide of entrained with, obtains regeneration lye.The regenerating alkali being discharged by anti-extraction unit
Liquid is recycled back to caustic wash unit and participates in desulfuration of liquefied gas process.
Selected liquefied gas is derived from wuhan petrochemical industry, and volume basis composition is as shown in table 1.
Table 1: liquefied gas hydro carbons volume basis composition
| N-alkane/% | Isoparaffin/% | Alkene/% | |
| C2 | 2.35 | 0 | 1.05 |
| C3 | 44.66 | 0 | 15.96 |
| C4 | 15.73 | 5.89 | 12.87 |
| C5 | 0 | 1.49 | 0 |
The method analysis that acid mercaptan total amount in above-mentioned liquefied gas is provided using SH/T 0222-92, the group of acid mercaptan
It is measured at using GC-SCD chromatography (PONA column).The quality group of surveyed mercaptan total amount becomes methyl mercaptan and accounts for 70.3%, and ethyl mercaptan accounts for
24.4%, propanethiol accounts for 5.3%.
Caustic wash unit and two-phase mixtures reactor used by anti-extraction unit are as depicted in figs. 1 and 2.Two-phase mixtures reaction
It include 11 groove structures in device, for caustic wash unit, the liquefied gas containing mercaptan enters two-phase mixtures via reactor inlet
In the distributing chamber of reactor, and mixing runner is entered by the entrance of mixing runner.Concentration is the NaOH aqueous solution of 15 weight %
Drop, which is formed, through distribution hole by cavity unit enters mixing runner, and the cross section of the cavity unit perpendicular to lye flow direction
Product is 280mm2, the cross-sectional area perpendicular to the mixing runner of sulfur-bearing lighter hydrocarbons flow direction is 3mm2, the length for mixing runner is
1000mm.The quantity of the distribution hole of the bottom of each groove structure is 4, and distribution hole depth is 1.0mm, according to lye in cavity
Flow direction in unit, the aperture of each distribution hole are respectively 0.9mm, 1.0mm, 1.1mm and 1.2mm, two neighboring distribution
The centre distance in hole is 23mm.Before entering mixing runner, the flow direction of liquefied gas and lye is adverse current, cavity unit
One end be closed end.Caustic wash unit is in such a way that two two-phase mixtures reactors are used in series, according to logistics direction, first
Temperature in grade two-phase mixtures reactor is 50 DEG C, pressure 1.2MPa；Temperature in the two-phase mixtures reactor of the second level is 50
DEG C, pressure 0.8MPa.
Apparent velocity of the liquefied gas in the inlet of mixing runner is 6m/s, and lye introduces the inlet of pipe in dispersed phase
Apparent velocity is 0.8m/s, and the content of mercaptan sulfur is 1000ppm in liquefied gas.Liquefied gas fills in mixing runner with lye two-phase
Enter collecting chamber after dividing mixing mass transfer, and draw reactor from reactor outlet, is separated into subsequent separation equipment.
After being separated by the fluid that first order two-phase mixtures reactor flows out, it is anti-that liquefied gas enters second level two-phase mixtures
Device (second level two-phase mixtures reactor is identical as the size of the first order two-phase mixtures reactor) is answered to continue to take off
Sulphur, by liquid of the fluid of second level two-phase mixtures reactor discharge after just dividing the desulfurization obtained after separation with sedimentation unit
Change air-flow and goes out reaction system.In liquefied gas after resulting desulfurization, the content of mercaptan sulfur is 3ppm, and desulfurization degree is 99.7 weights
Measure %.
Also be used in series using two two-phase mixtures reactors in anti-extraction unit, and the structure of two-phase mixtures reactor with
The structure snd size of the two-phase mixtures reactor of caustic wash unit are all the same.The temperature of first order two-phase mixtures reactor is 50 DEG C,
Pressure is 1.0MPa, and the temperature of second level two-phase mixtures reactor is 50 DEG C, pressure 0.6MPa.Lye is in mixing flow channel entry point
The apparent velocity at place is 6m/s, and gasoline is 0.6m/s in the apparent velocity that dispersed phase introduces the inlet of pipe.Lye after desulfurization
In be entrained with disulphide, sulfur content 325ppm.The sulfur content in regeneration lye obtained after anti-extraction unit is
12ppm。
Due to not adding any surface reactive material that can drop interfacial tension in reaction system, this height of system is utilized
The characteristics of interfacial tension, liquefied gas and lye split-phase can be clarified rapidly in precipitation apparatus, and occur without emulsion layer.
Embodiment 2
The present embodiment carries out lighter hydrocarbons desulfurization using two-phase mixtures reactor of the present invention, specifically as follows:
The method of lighter hydrocarbons desulfurization in the present embodiment is similar to embodiment 1, also includes 11 in two-phase mixtures reactor
Groove structure, except that:
Lighter hydrocarbons in the present embodiment are light petrol, and it is anti-to only have a two-phase mixtures in caustic wash unit and anti-extraction unit
Answer device.
Selected light petrol is derived from Jiujiang petrochemical industry, and hydro carbons volume basis composition is as shown in table 2.
Table 2: light petrol hydro carbons volume basis composition
| N-alkane/% | Isoparaffin/% | Alkene/% | Diene/% | |
| C4 | 2.141 | 0.978 | 5.237 | 0 |
| C5 | 13.368 | 41.388 | 29.821 | 0.039 |
| C6 | 0 | 5.889 | 1.140 | 0 |
The method measurement that acid mercaptan total amount in light petrol is provided using GB/T 1792-1988, the composition of acid mercaptan
It is measured using GC-SCD chromatography (PONA column).The quality group of surveyed mercaptan total amount becomes methyl mercaptan and accounts for 8.89%, and ethyl mercaptan accounts for
66.7%, propanethiol accounts for 24.4%.
In caustic wash unit: 3 distribution holes are provided in the bottom of each groove structure, distribution hole depth is 1.1mm, and
According to flow direction of the lye in cavity unit, the aperture of each distribution hole is respectively 1.05mm, 0.8mm and 0.6mm, adjacent
The centre distance of two distribution holes is 25mm.Cross-sectional area perpendicular to the cavity unit of lye flow direction is 280mm2,
Cross-sectional area perpendicular to the mixing runner of sulfur-bearing lighter hydrocarbons flow direction is 3mm2, the length for mixing runner is 500mm.Two-phase is mixed
Closing the temperature in reactor is 45 DEG C, pressure 1.2MPa.Light petrol is 8m/s, alkali in the apparent velocity of mixing flow passage entry
Liquid is 0.48m/s in the apparent velocity that dispersed phase introduces the inlet of pipe, and the content of mercaptan sulfur is 78ppm in light petrol.
By in the light petrol of caustic wash unit, the content of mercaptan sulfur is 3.5ppm, desulfurization degree is 95.5 weight %.
In anti-extraction unit: the two-phase mixtures of the caustic wash unit in the structure and the present embodiment of two-phase mixtures reactor are anti-
Answer device structure snd size all the same.The temperature of two-phase mixtures reactor is 52 DEG C, pressure 1.0MPa.Lye is in mixing runner
The apparent velocity of inlet is 7m/s, and gasoline is 2m/s in the apparent velocity that dispersed phase introduces the inlet of pipe.Alkali after desulfurization
Disulphide, sulfur content 48ppm are entrained in liquid.The sulfur content in regeneration lye obtained after anti-extraction unit is
3ppm。
Remaining is in the same manner as in Example 1.
Embodiment 3
The present embodiment carries out lighter hydrocarbons desulfurization using two-phase mixtures reactor of the present invention, specifically as follows:
The method of lighter hydrocarbons desulfurization in the present embodiment is similar to embodiment 2, except that:
In caustic wash unit: according to flow direction of the lye in cavity unit, the aperture of each distribution hole is respectively
1mm, 0.7mm and 0.4mm, distribution hole depth are 1mm, and the centre distance of two neighboring distribution hole is 27mm.Perpendicular to lye
The cross-sectional area of the cavity unit of flow direction is 280mm2, perpendicular to the cross section of the mixing runner of sulfur-bearing lighter hydrocarbons flow direction
Product is 6mm2, the length for mixing runner is 1000mm.Temperature in two-phase mixtures reactor is 50 DEG C, pressure 1.2MPa.Gently
Gasoline is 8m/s in the apparent velocity of mixing flow passage entry, and lye is in the apparent velocity that dispersed phase introduces the inlet of pipe
1.25m/s.The present embodiment uses light petrol same as Example 2 as sulfur-bearing lighter hydrocarbons, and addition ethyl mercaptan makes thereto
The content for obtaining mercaptan sulfur in the light petrol of the present embodiment is 1000ppm.
By in the light petrol of caustic wash unit, the content of mercaptan sulfur is 14ppm, desulfurization degree is 98.6 weight %.
In anti-extraction unit: the alkali cleaning list in the structure and the present embodiment of the two-phase mixtures reactor in anti-extraction unit
The two-phase mixtures structure of reactor and size of member are all the same.The temperature of two-phase mixtures reactor is 52 DEG C, pressure 1.1MPa.Alkali
Apparent velocity of the liquid in the inlet of mixing runner is 6m/s, and gasoline is in the apparent velocity that dispersed phase introduces the inlet of pipe
3m/s.Disulphide, sulfur content 560ppm are entrained in lye after desulfurization.The regenerating alkali obtained after anti-extraction unit
Sulfur content in liquid is 45ppm.
Remaining is in the same manner as in Example 2.
Comparative example 1
This comparative example is carried out using method similar to Example 2, the difference is that the two-phase mixtures of this comparative example react
Device is packed extraction tower, and tower diameter 250mm, tower height 2m, bed stuffing height 1.5m, filler is to dissipate heap Raschig ring, Raschig ring
Diameter is 16mm.The processing capacity of packed tower is identical as the ability of two-phase mixtures reactor used in embodiment 1.
Remaining is in the same manner as in Example 2.
As a result: the separating property data of the extraction tower of the de- and anti-extraction unit of the extraction tower of caustic wash unit and 2 phases of implementation
Seemingly, but continuous phase load of the two-phase mixtures reactor provided by the invention on unit cross-sectional area is equivalent to extraction tower
1500 times or more, fully demonstrate that two-phase mixtures reactor volume provided by the invention is small, processing capacity is big, mass transfer in contrast
High-efficient feature.
Comparative example 2
This comparative example is carried out using method similar to Example 2, the difference is that the two-phase mixtures of this comparative example react
Device be concatenated two identical micro- blenders of T-type (runner i.e. where lye with mix runner directly intersect vertically without
The structure of reflux type), the mixing runner cross-sectional area of each mixer is 4mm2, dispersed phase flow diameter is 2mm.Each T
The processing capacity of the micro- blender of type mixes runner using one of two-phase mixtures reactor of the present invention with embodiment 2
Processing capacity is identical.
Remaining is in the same manner as in Example 2.
As a result: the desulfurization degree of light petrol is 72 weight %, has fully demonstrated two-phase mixtures provided by the invention in contrast
The high feature of reactor mass-transfer efficiency.
It can be seen that from the result of the embodiment of the present invention 1-3 and comparative example 1-2 and reacted using two-phase mixtures of the invention
When device carries out lighter hydrocarbons desulfurization, the desulfurization effect of acquirement is obviously better than the desulfurization effect of the prior art.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (17)
1. a kind of two-phase mixtures reactor, which is characterized in that the two-phase mixtures reactor includes that reactor inlet, reactor go out
Mouth, reactor tank body (3) and reaction module (4), the outer surface of the reaction module is provided at least two groove structures, described
The protrusion side wall (9) of groove structure is connect with the inner wall of the reactor tank body, the groove structure and the reactor tank body
Inner wall between form mixing runner (6), the reaction module is internally provided with cavity unit (5), and the cavity unit is logical
It crosses and the distribution hole (8) of the bottom of groove structure of the reaction module is set is connected to the mixing runner, wherein the sky
The setting of the entrance of chamber unit so that flow direction of the fluid in the cavity unit in the flowing mixed in runner
It is contrary；The outlet of the entrance of the mixing runner and the mixing runner respectively with the reactor inlet and described react
Device outlet keeps connection.
2. two-phase mixtures reactor according to claim 1, which is characterized in that the two-phase mixtures reactor further wraps
Collecting chamber and distributing chamber are included, the reactor inlet is connected to the entrance of the mixing runner, the mixed flow through the distributing chamber
The outlet in road is connected to the reactor outlet through the collecting chamber.
3. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that the inner wall of the reactor tank body encloses
At space be at least one of cylindrical shape, Elliptic Cylinder shape, cube-shaped and rectangular-shape.
4. two-phase mixtures reactor according to claim 3, which is characterized in that the inner wall of the reactor tank body surrounded
Space is cylindrical shape.
5. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that the bottom of each groove structure
Distribution hole number it is identical or different, and the number of the distribution hole of the bottom of each groove structure is each independently 1-
100.
6. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that the aperture of each distribution hole is
0.1-2mm。
7. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that according to the stream in the cavity unit
The aperture of the flow direction of body, the distribution hole is sequentially increased.
8. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that according to the stream in the cavity unit
The flow direction of body, the small 0.01-1mm in aperture of the adjacent distribution hole in the aperture ratio downstream of the distribution hole of upstream.
9. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that at the bottom of each groove structure
Portion, the distance of the central point of two neighboring distribution hole are 0.5-40mm.
10. two-phase mixtures reactor according to claim 9, which is characterized in that in the bottom of each groove structure,
The distance of the central point of two neighboring distribution hole is 1-30mm.
11. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that the depth of the distribution hole is 0.1-
3mm。
12. two-phase mixtures reactor according to claim 11, which is characterized in that the depth of the distribution hole is 0.3-
2.5mm。
13. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that be provided with fibre in the mixing runner
Tie up silk.
14. two-phase mixtures reactor according to claim 13, which is characterized in that the fiber filament is linear or spiral
Shape.
15. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that the cavity unit it is open at one end
For fluid inlet, the other end is closed end.
16. two-phase mixtures reactor according to claim 1 or 2, which is characterized in that the protrusion side wall of the groove structure
Connection type between the inner wall of the reactor tank body, which is selected from, to be welded to connect, is threadedly coupled, expanded joint, stings seam connection, be glued
At least one of connected with blind rivet.
17. two-phase mixtures reactor described in any one of claim 1-16 in liquid liquid two-phase or gas/liquid two-phase mixtures and
Application in reaction.
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| WO2010119624A1 (en) * | 2009-04-17 | 2010-10-21 | 日曹エンジニアリング株式会社 | Tubular flow type reactor |
| CN204395969U (en) * | 2014-12-06 | 2015-06-17 | 中国石油化工股份有限公司 | Novel rotary bed bioreactor |
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| WO2010119624A1 (en) * | 2009-04-17 | 2010-10-21 | 日曹エンジニアリング株式会社 | Tubular flow type reactor |
| CN101757884A (en) * | 2010-02-10 | 2010-06-30 | 浙江工业大学 | Novel gas-liquid reactor |
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