CN106433738A - Reduced pressure distillation experimental device for high-viscosity oil - Google Patents
Reduced pressure distillation experimental device for high-viscosity oil Download PDFInfo
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- CN106433738A CN106433738A CN201610962704.6A CN201610962704A CN106433738A CN 106433738 A CN106433738 A CN 106433738A CN 201610962704 A CN201610962704 A CN 201610962704A CN 106433738 A CN106433738 A CN 106433738A
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- bowl
- backflow
- oil gas
- condensing
- rectifying column
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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
- C10G7/00—Distillation of hydrocarbon oils
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
- B01D3/106—Vacuum distillation with the use of a pump for creating vacuum and for removing the distillate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- 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
- C10G7/00—Distillation of hydrocarbon oils
- C10G7/06—Vacuum distillation
-
- 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
- C10G7/00—Distillation of hydrocarbon oils
- C10G7/12—Controlling or regulating
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a reduced pressure distillation experimental device for high-viscosity oil. The device comprises a distillation kettle, a heater used for heating the distillation kettle, a rectifying tower connected with an outlet of the distillation kettle, a condenser connected with an outlet of the rectifying tower, and a fraction receiver connected with an outlet of the condenser, wherein a porous foam breaking net is arranged on a channel used for connecting an inner cavity of the distillation kettle and an inner cavity of the rectifying tower. According to the reduced pressure distillation experimental device, the porous foam breaking net is arranged on the channel used for connecting the inner cavity of the distillation kettle and the inner cavity of the rectifying tower, and the excessive foam generated in a distillation process is blocked and suppressed by the porous foam breaking net, so that the phenomenon that a great deal of foam rushes into the rectifying tower upwards can be avoided; furthermore, an oil-gas flow equalizing plate is capable of effectively changing the direction of ascending airflow, so that the situation that the airflow directly brings all the oil into the condenser due to a sudden increase of pressure, so that the experimental requirements cannot be realized, and the experimental effect is finally influenced is avoided. The reduced pressure distillation experimental device can be applied to an oil distillation experiment.
Description
Technical field
The present invention relates to laboratory oil product retort field, more particularly to a kind of vacuum distillation reality for high viscosity oil
Experiment device.
Background technology
By distillation test being carried out to fluid oil, its each fraction can be cut, obtain corresponding narrow fraction
Yield, and its boiling range data are obtained.Therefore the distillation test of fluid oil not only can obtain production for petroleum refining enterprise
The master data of processing, and evaluate the important indicator of oil product performance.Existing fluid oil products distillation test device master
There are true boiling point distillation instrument, Engler distillation instrument and kirschner vacuum distillation instrument, they may be conveniently used evaluation crude oil, fuel
Oily, lubricating oil and decompression residuum etc., but the distillation for high viscosity poor residuum, Colophonium and slurry oil is but difficult to.Than
Reflux ratio as business-like true boiling point distillation instrument is adjusted and is generally controlled using electromagnetism balancing point, higher acid in poor residuum
Content is easily corroded the little iron block on backflow head and so that balancing point is failed.And Engler distillation instrument and kirschner vacuum distillation instrument often can only
Carry out simple Measurement of distilled process, it is impossible to realize the accurate cutting of narrow fraction.
The problem for particularly perplexing be these experimental provisions above-mentioned in still-process, due to high-viscosity oil product surface relatively
Thick, during heating, bottom viscosity first diminishes, and surface does not soften completely, and in the larger air pressure of bottom portion accumulation.And
Outlet due to distillating still can form some foams regularly, these foams through heating and the drive of air-flow be easy to
On pour in rectifying column, experiment is brought greater impact, or even causes abnormal phenomenas such as " rushing tower ".This phenomenon is not only tested
Obtain and stop at once, and cause whole the failure of an experiment, because the distillate of the rectifying column that goes out again cannot accurately calculate weight
Amount.
Content of the invention
In order to solve the above problems, it is an object of the invention to provide a kind of vacuum distillation for high viscosity oil is tested
Device, can effectively prevent foam from rushing tower.
The technical solution adopted in the present invention is：
A kind of vacuum distillation experimental provision for high viscosity oil, including distillating still, the heater for heating for distillating still, connection
The rectifying column of distillating still outlet, the condenser of connection rectifying column outlet, the fraction receptor of connection condensator outlet, connection distillation
Kettle inner chamber is provided with cellular type demister with the passage of rectifying column inner chamber, is provided with oil between the oil gas vent of rectifying column and condenser
Gas homogenizing plate.
As a further improvement on the present invention, the distillating still top is provided with outlet of the diameter not less than 100mm, distillating still
The entrance of the periphery of outlet and rectifying column is provided with the flange part for complementing one another, and the entrance of rectifying column is by flange part connection distillation
The outlet of kettle.
As a further improvement on the present invention, the condenser includes condensing tube and condensing reflux pipe, and the rectifying column is
Column structure, the periphery of rectifying column oil gas vent is provided with backflow and receives bowl, and backflow receives bowl and is located at returning for condensing reflux pipe
At flow liquid whereabouts, backflow receives bowl and is provided with condensation interface tube, and condensing tube is connect by condensing the interface tube connection backflow
Receive bowl.
As a further improvement on the present invention, the backflow receives bowl and is provided with drain pipe, and drain pipe is configured with draining
Valve.
As a further improvement on the present invention, the backflow is received in bowl and is provided with liquid phase partition member, and the liquid phase is divided
The condensation for being separated into connection condensation interface tube in part is by backflow reception bowl is discharged chamber and discharges chamber separation with condensing
Backflow sap cavity, inside the backflow sap cavity connection rectifying column.
As a further improvement on the present invention, the condensing reflux pipe includes oil gas vent bowl, liquid-phase reflux pipe, the oil
Gas exports bowl back-off shape, and the larger bottom opening of its bore is relative with backflow reception bowl, the entrance connection of liquid-phase reflux pipe
In the less open top in oil gas vent the rim of a bowl footpath, oil gas homogenizing plate is fixed in oil gas vent bowl, the oil gas homogenizing plate
Positioned at the underface of liquid-phase reflux tube inlet and oil gas homogenizing plate projected area in the horizontal plane be more than liquid-phase reflux tube inlet
Projected area in the horizontal plane.
As a further improvement on the present invention, the oil gas homogenizing plate towards the top surface of liquid-phase reflux tube inlet be by center
To the cambered surface that surrounding gradually has a down dip, or the oil gas homogenizing plate is the low spherical crown shape of middle high surrounding or umbrella shape.
As a further improvement on the present invention, the condensing tube includes the two-stage nitration condensation being connected in parallel on fraction receptor
Pipe and three sections of condensing tubes, the arrival end connection condensation interface tube of the two-stage nitration condensing tube, the arrival end of three sections of condensing tubes is even
Connect the oil gas vent of condensing reflux pipe.
As a further improvement on the present invention, on the export pipeline of the condensing reflux pipe, relief valve is connected to.
As a further improvement on the present invention, the fraction receptor includes epimere receiver and hypomere receiver, described
Epimere receiver connects the rectifying column, and the hypomere receiver connects epimere reservoir by the valve module on pipeline and pipeline
Tank, the hypomere receiver is made up of Pyrex material.
The invention has the beneficial effects as follows：The present invention is provided with cellular type on connection passage of the distillating still inner chamber with rectifying column inner chamber
Demister, the excessive foam produced by still-process can be intercepted by cellular type demister and be suppressed, a large amount of so as to avoid
Foam is poured in rectifying column upwards, additionally, oil gas homogenizing plate can effectively change the direction of ascending air, prevents pressure from increasing suddenly
When, air-flow is directly all brought into the requirement that cannot realize testing in condenser by oil product, affects final experiment effect.
Description of the drawings
The present invention is further described with embodiment below in conjunction with the accompanying drawings.
Fig. 1 is the front view of experimental provision；
Fig. 2 is the rearview of experimental provision；
Fig. 3 is the schematic diagram of distillating still；
Fig. 4 is the outside schematic diagram of rectifying column；
Fig. 5 is the internal structure schematic diagram of rectifying column；
Fig. 6 is the top view of rectifying column；
Fig. 7 is the outside schematic diagram of condensing reflux pipe；
Fig. 8 is the internal structure schematic diagram of condensing reflux pipe；
Fig. 9 is the left view of fraction receptor；
Figure 10 is the front view of fraction receptor；
Figure 11 is experimental provision still-process schematic diagram.
Specific embodiment
The vacuum distillation experimental provision for high viscosity oil with reference to shown in Fig. 1, including distillating still 1, adds for distillating still 1
The heater 2 of heat, connects the rectifying column 3 of the outlet of distillating still 1, the condenser of the connection outlet of rectifying column 3, connection condensator outlet
Fraction receptor 4.With reference to Fig. 5 and with reference to Fig. 1 and Fig. 2, distillating still 1 and rectifying column 3 are respectively provided with inner chamber, wherein connect distillating still 1
Inner chamber is provided with cellular type demister 5 with the passage of 3 inner chamber of rectifying column.Excessive foam produced by still-process can be by cellular type
Demister 5 is intercepted and is suppressed, and is poured in rectifying column 3 upwards so as to avoid a large amount of foams, affects final experiment effect.
With reference to Fig. 3, described distillating still 1 is designed for closing in type, and the bottom of distillating still 1 is ellipsoidal head 11, oval
Cylindrical stack shell 12 being welded on end socket 11, welding concentric reducer 13 on cylindrical stack shell 12, the top of concentric reducer 13 is distillating still 1
Outlet, has flat mouth flange 14 in the peripheral solder of concentric reducer 13.What in embodiment, 1 kettle mouth of distillating still namely distillating still 1 were exported is straight
Footpath should be not less than 100mm, no dead angle when this larger-size kettle mouth is conducive to bottoms to discharge and clean.
With reference to Fig. 4 to Fig. 6, described rectifying column 3 is column, in its bottom welding flat mouth flange 34, the flat mouth flange 34
It is bolted with flat mouth flange 14 on distillating still 1, so as to facilitate both dismountings.
Concentric reducer 35 is welded on flat mouth flange 34 on rectifying column 3, the bottom opening of the concentric reducer 35 is with diameter greater than top
It is open, and the bottom opening of the concentric reducer 35 is docked with the top exit of distillating still 1, described cellular type demister 5 is fixed on
Inside concentric reducer 35.35 upper end weld filler section 36 of concentric reducer, fills filler inside packing section 36, and filler bottom plate washer is arranged at its bottom
37, filler top plate washer 38 is removably installed by bolt in the exit at packing section top, with easy disassembly, is easy to taking for filler
Go out.
The outlet of packing section 36 can be regarded as the outlet of rectifying column 3, be fixedly connected with backflow in the periphery of packing section 36
Liquid receives bowl 31, and backflow receives the top of bowl 31 and is connected to flat mouth flange 311.With reference to Fig. 7 and Fig. 8, described condenser is at least
Including condensing reflux pipe 6, condensing reflux pipe 6 is connected at backflow reception bowl 31 by being located at the flat mouth flange 65 of itself bottom
Flat mouth flange 311, receives a part of oil gas from rectifying column 3, and produces backflow by way of condensation and fall.Above-mentioned
Backflow is received at whereabouts of the bowl 31 just at 6 backflow of condensing reflux pipe.
With continued reference to Fig. 4 to Fig. 6, condenser also includes condensing tube, and the backflow receives bowl 31 and is provided with condensing tube
Interface 32, condensing tube connects backflow reception bowl 31 by condensing interface tube 32, and partial reflux liquid is arranged to Fig. 1 and Tu
Fraction receptor 4 shown in 2.In order to control backflow to enter the flow of fraction receptor 4, backflow is received in bowl 31 and is provided with liquid
Phase partition member, liquid phase partition member backflow is received be separated in bowl 31 connection condensation interface tube 32 condensation discharge chamber with
And discharge, with condensation, the backflow sap cavity that chamber separates.Inside backflow sap cavity connection rectifying column 3, partial reflux liquid is thereby returned to rectifying column
In 3, remainder is discharged in chamber in condensation and flows to fraction receptor 4.In embodiment, liquid phase partition member can be two block weldings
The liquid phase plate 312 on bowl is received in backflow, two liquid phase plates, 312 angle in 90 ° is so as to be divided into 1/4 volume by backflow reception bowl
Condensation discharge the backflow sap cavity of chamber and 1/4 volume.
Backflow receives bowl 31 and is also circumscribed with drain pipe 33, and drain pipe 33 is configured with drain valve.Some need the oil of distillation
Moisture content can be contained in product, due to the backflow effect of condensing reflux pipe 6 and the sealing requirements of device, these water can filled always
Put interior circulation and be difficult to discharge.Pass through drain pipe 33 in embodiment, can be used to, when distilling initial, discharge and be mixed in residual oil on a small quantity
Moisture content, to ensure the stationarity in follow-up still-process.In addition, being welded with oil temperature thermocouple sheath in kettle on concentric reducer 35
351st, kettle top interior temperature thermocouple sheath 352, installs two kinds of thermocouples to facilitate, and monitors the temperature of rectifying column 3, in packing section 36
Middle part also is provided with temperature thermocouple sheath 361 in post, installs corresponding thermocouple to facilitate, and monitors the temperature at 3 middle part of rectifying column.
With reference to Fig. 7 and Fig. 8, in embodiment, described condensing reflux pipe 6 includes flat mouth method, 65, oil gas vent bowl 61, liquid
Phase return duct 62.Oil gas vent bowl 61,61 back-off shape of oil gas vent bowl, the larger bottom of its bore are welded in 65 upper end of flat mouth flange
Portion's opening is relative with backflow reception bowl 31, and the entrance of liquid-phase reflux pipe 62 is connected to the less top of 61 bore of oil gas vent bowl
On opening, 62 outer layer of liquid-phase reflux pipe is cooling water layer 66.Oil gas vent mercurial thermometer is welded with oil gas vent bowl 61 respectively
Sleeve pipe 611 and oil gas vent thermocouple sheath 612, oil gas vent mercurial thermometer sleeve pipe 611 and oil gas vent thermocouple sheath
Be respectively equipped with mercurial thermometer and thermocouple on 622, for monitor rectifying column outlet state, while arrange mercurial thermometer and
At the two of thermocouple temperature measurement, mercurial thermometer and thermocouple temperature measurement, temperature detection is to ensure the accuracy of outlet temperature.Liquid phase is returned
The top of flow tube 62 is the oil gas vent of condensing reflux pipe 6.
Further, with reference to Fig. 1, the oil gas vent of liquid-phase reflux pipe 62 is further connected with relief valve 64, and its set-pressure is 0.4
MPa, as pipeline is easily clogged in the distillation such as residual oil and slurry oil sometimes, particularly in some modification slurry oil scientific experiments, unexpected
Factor is present, and therefore arranges the safety that relief valve 64 ensure that operator.
Preferably, with reference to Fig. 8, in oil gas vent bowl 61, oil gas homogenizing plate 63 is provided with, the oil gas homogenizing plate 63 is located at liquid
The underface of 62 entrance of phase return duct and the projected area in the horizontal plane of oil gas homogenizing plate 63 are more than 62 entrance of liquid-phase reflux pipe
Projected area in the horizontal plane.
Oil gas homogenizing plate 63 can not only effectively change the direction of ascending air, and when preventing pressure from increasing suddenly, air-flow is by oil
The requirement that product are directly taken condensing reflux pipe out of and cannot realize testing, as shown in the solid line of in figure and arrow, air-flow needs to bypass
Oil gas homogenizing plate 63 could continue to ascend into liquid-phase reflux pipe 62, reach the effect of uniform rising；And liquid can prevented
The condensed fluid of phase return duct 62 is along in the direct drip back rectifying column 3 of tube wall.In embodiment, the backflow of liquid-phase reflux pipe 62 along
The surrounding dispersion of oil gas homogenizing plate 63 is fallen, and as shown in broken lines, and uniform flow Huis flow liquid is received in bowl.
Oil gas homogenizing plate 63 can have various shapes, the top surface for being such as directed towards 62 entrance of liquid-phase reflux pipe be from center to
The cambered surface that surrounding gradually has a down dip, or oil gas homogenizing plate 63 is the low spherical crown shape of middle high surrounding or umbrella shape.
With reference to Fig. 1, described condensing tube include the two-stage nitration condensing tube 71 being connected in parallel on fraction receptor 4 and three sections cold
Solidifying pipe 72, the arrival end connection condensation interface tube 32 of two-stage nitration condensing tube 71, the arrival end connection condensing reflux of three sections of condensing tubes 72
The oil gas vent of pipe 6.The internal layer of two-stage nitration condensing tube 71 and three sections of condensing tubes 72 is oil-gas Layer, and outer layer is cooling water layer.
With reference to Fig. 9 and Figure 10, in embodiment, fraction receptor 4 includes epimere receiver 41 and hypomere receiver 42, epimere
Receiver 41 is stainless steel, and hypomere receiver 42 is Pyrex material.Epimere receiver 41 is circumscribed with vacuum adapter 43,
Vacuum adapter 43 is connected with vacuum pump described later, and vacuum adapter 43 is connected with hypomere receiver 42 by pipeline, and
The pipeline is provided with stop valve 44, and hypomere receiver 42 is circumscribed with atmospheric valve 45, and the bottom of hypomere receiver 42 is provided with discharge opeing
Valve 46, is additionally provided with a stop valve 47 between epimere receiver 41 and hypomere receiver 42.Hypomere receiver 42 is Pyrex
Material, to facilitate observation to collect the volume of fraction.During fraction switching, stop valve 47 and stop valve 44 is closed, while opening logical big
Air valve 45, you can the fraction for receiving i.e. in hypomere receiver 42 is discharged, while not affecting being normally carried out for vacuum distillation.
Preferably, with reference to Fig. 2, experimental provision also includes vacuum pump 8 and vacuum buffer tank 81, and vacuum pump 8 is used for as device
Vacuum condition is provided and connects above-mentioned vacuum adapter 43, vacuum buffer tank 81 is connected to the suction inlet of vacuum pump 8 by pipeline,
Vacuum buffer tank outer layer can lead to low-temperature cooling water, for the non-condensing gas of cooling segment, reduce and do not coagulate gas entrance vacuum pump, prolong
The service life of long pumping fluid.
Can be wall type heating furnace 21 with reference to the heater 2 in Fig. 1 and Fig. 2 embodiment, wall type heating furnace 21 can be by electricity
Dynamic lifting platform 22 is moved up and down and is vertically accessed in distillating still 1 so that distillating still 1 is located inside wall type heating furnace 21, is conducive to
The fast cooling for removing with distillating still 1 of heating furnace.Wall type heating furnace 21 is using two sections independent heating and temperature control, and highest can
600 DEG C are heated to, and outermost layer wall temperature is less than 80 DEG C, using high temperature resistant cloud bussed supply, electric wire is prevented because of Long Term Contact temperature
The higher furnace wall of degree and aging.
Experimental provision in embodiment is configured with and electric control cabinet (not shown), and the electrical control cabinet is provided with supply lines
Road, temp controlled meter, touch screen and controlling switch.Employing graphic control panel on switch board is host computer, and temp controlled meter is slave computer
The controllability of instrument when double control system ensure that part instrument malfunction.
Assay device in embodiment is on an instrument stand 9, and the instrument stand 9 carries four universal caster wheels, side
Just move, various instrument, the electric wire of instrument are placed in the cupboard of the instrument stand back side using lineback mode, make assay device clean and tidy
Attractive in appearance.
Hereinafter the work process of experimental provision is illustrated.
1, oil sample loads." decline " button of lifting motor is pressed in electric control cabinet, is made wall type heating furnace 21 and is steamed
Evaporate kettle 1 to be kept completely separate, distillating still 1 is unloaded, if unclean toward kettle in distillating still 1, need to first clean and add the oil to be distilled for having measured
Sample, cumulative volume does not exceed the 2/3 of the maximum volume of distillating still 1.
2, distillating still 1 is installed.First wall type heating furnace 21 is moved apart electric lifting platform 22；Then the steaming of oil sample has been added
Evaporating kettle 1 to place on 22 face of electric lifting platform, 1 pop-up of " rising " button distillating still of lifting motor is pressed to just two panels flat mouth method
The position that orchid contacts, tightens whole nuts.Electric lifting platform 22 is finally fallen, wall type heating furnace 21 is put electric lifting platform
In 22, simultaneously distillating still 1 is inserted in pop-up.
3, airtight test.First confirm that tapping valve 46 and valve 701,801 are closed, if being not turned off, must
Must close.Compressed air is accessed by drain pipe 33, valve 801 is opened, make instrument internal that 0.1 MPa is boosted to, close valve
801.Pressure is observed by pressure gauge and reduces situation, technological requirement is leaked<5 Pa/h, that is, think that air-tightness reaches requirement.If gas
Close property is not up to standard, need to first check air leakage point and take corresponding measure to exclude gas leakage.
4, heat up and first prepare.First check whether each valve is in closing or the open mode of technological requirement, check control electricity
Whether the power supply of device cabinet is normal, checks whether each temp controlled meter, pressure gauge and touch screen normally show, checks whether condenser is complete
Portion connects cooling water.
5, start distillation.By technological requirement, the heating-up temperature of tower reactor is set.During vacuum distillation, when in kettle, oil temperature shows
About 90 DEG C, start vacuum pump 8, and the valve 701 being connected with instrument before guaranteeing pump is opened.
6, the flow direction of still-process air-flow is as follows：With reference to Figure 11, the oil in distillating still 1 become gas rise through cellular type break
Foam net 5, then proceedes to rise through packing section 36；A part of oil gas enters condensation in two-stage nitration condensing tube 71 and becomes liquid oil, it
Flowed in the epimere receiver 41 of fraction receptor afterwards, another part oil gas rises to condensing reflux pipe 6.In condensing reflux pipe 6
Oil gas be partly in three sections of condensing tubes 72 and become liquid oil and flow into epimere receiver 41, another part condensing reflux is extremely
Backflow receives bowl 31, and backflow receives the condensed fluid of bowl 31 has 1/4 inflow two-stage nitration condensing tube 71,3/4 to return in rectifying column 3；
In epimere receiver 41, oil is downwardly into hypomere receiver 42.
7, the hypomere receiver 42 of fraction receptor 4 is observed, when the first drop of liquid is dripped, at this moment corresponding temperature is first
Evaporate a little, as the starting point of distillation.Every certain temperature range, the distillate for being received in the range of corresponding temperature is just released.Evaporate
Point release method be：Stop valve 47 and the stop valve 44 of fraction receptor 4 is closed, is at this moment cut off with vacuum section, then beat
Open atmos-valve 45 so that the pressure in hypomere receiver 42 is balanced with external atmosphere pressure, it is right to release by opening tapping valve 46
The distillate that answers.During switchback vacuum state, shutoff valve tapping valve 46 and atmospheric valve 45, then open stop valve 47 and cut successively
Only valve 44.
8, the temperature of wall type heating furnace 21 is constantly raised, until distillation terminates.When there is obvious oil breakdown phenomenon,
When hypomere receiver 42 can be observed white smoke, heating should be stopped immediately.
9, after the completion of distillation, stop heating.When less than 120 DEG C are down to Deng distillation temperature in the kettle, close vacuum pump.Instrument
After lowering the temperature completely, cooling water is closed.
10, distillating still being unloaded by step 1, pours out residual liquid and measured, and clean distillating still.
11, after the completion of experiment, close valve power supply.
The above is the preferred embodiment of the present invention, and which does not constitute limiting the scope of the invention.
Claims (10)
1. a kind of vacuum distillation experimental provision for high viscosity oil, including distillating still (1), heat for distillating still (1) plus
Hot device (2), connect distillating still (1) export rectifying column (3), connection rectifying column (3) export condenser, connection condensator outlet
Fraction receptor (4), it is characterised in that：Connection distillating still (1) inner chamber is provided with cellular type with the passage of rectifying column (3) inner chamber and breaks
Foam net (5), is provided with oil gas homogenizing plate (63) between the oil gas vent of rectifying column (3) and condenser.
2. the vacuum distillation experimental provision for high viscosity oil according to claim 1, it is characterised in that：The distillation
Kettle (1) top is provided with outlet of the diameter not less than 100mm, and the periphery that distillating still (1) is exported and the entrance of rectifying column (3) are provided with
The flange part for complementing one another, the entrance of rectifying column (3) connects the outlet of distillating still (1) by flange part.
3. the vacuum distillation experimental provision for high viscosity oil according to claim 1, it is characterised in that：The condensation
Device includes condensing tube and condensing reflux pipe (6), and described rectifying column (3) are that column structure, the periphery of rectifying column (3) oil gas vent sets
Backflow is had to receive bowl (31), backflow receives bowl (31) and is located at the backflow whereabouts of condensing reflux pipe (6), and backflow is received
Bowl (31) is provided with condensation interface tube (32), and condensing tube receives bowl (31) by condensing interface tube (32) the connection backflow.
4. the vacuum distillation experimental provision for high viscosity oil according to claim 3, it is characterised in that：The backflow
Liquid receives bowl (31) and is provided with drain pipe (33), and drain pipe (33) is configured with drain valve.
5. the vacuum distillation experimental provision for high viscosity oil according to claim 3, it is characterised in that：The backflow
Liquid is received in bowl (31) and is provided with liquid phase partition member, and the liquid phase partition member receives backflow in bowl (31) and is separated into connection
The condensation of condensation interface tube (32) is discharged chamber and is discharged the backflow sap cavity of chamber separation with condensation, and the backflow sap cavity connects rectification
Tower (3) is internal.
6. the vacuum distillation experimental provision for high viscosity oil according to claim 3 or 4 or 5, it is characterised in that：Institute
State condensing reflux pipe (6) include oil gas vent bowl (61), liquid-phase reflux pipe (62), oil gas vent bowl (61) back-off shape,
The larger bottom opening of its bore is relative with backflow reception bowl (31), and the entrance of liquid-phase reflux pipe (62) is connected to oil gas vent
In the less open top of bowl (61) bore, oil gas homogenizing plate (63) is fixed in oil gas vent bowl (61), and the oil gas all flows
Plate (63) is located at the underface of liquid-phase reflux pipe (62) entrance and oil gas homogenizing plate (63) projected area in the horizontal plane is more than
Liquid-phase reflux pipe (62) entrance projected area in the horizontal plane.
7. the vacuum distillation experimental provision for high viscosity oil according to claim 6, it is characterised in that：The oil gas
Homogenizing plate (63) is the cambered surface gradually being had a down dip to surrounding from center towards the top surface of liquid-phase reflux pipe (62) entrance, or the oil gas
Homogenizing plate (63) is the low spherical crown shape of middle high surrounding or umbrella shape.
8. the vacuum distillation experimental provision for high viscosity oil according to claim 3 or 4 or 5, it is characterised in that：Institute
Stating condensing tube includes the two-stage nitration condensing tube (71) that is connected in parallel on fraction receptor (4) and three sections of condensing tubes (72), described two
Arrival end connection condensation interface tube (32) of section condensing tube (71), the arrival end connection condensing reflux of three sections of condensing tubes (72)
The oil gas vent of pipe (6).
9. the vacuum distillation experimental provision for high viscosity oil according to claim 3 or 4 or 5, it is characterised in that：Institute
Relief valve (64) is connected on the export pipeline for stating condensing reflux pipe (6).
10. the vacuum distillation experimental provision for high viscosity oil according to claim 1 or 2 or 3 or 4 or 5, its feature
It is：Described fraction receptor (4) include epimere receiver (41) and hypomere receiver (42), and described epimere receiver (41) connect
The rectifying column (3) is connect, described hypomere receiver (42) connect epimere receiver (41) by the valve module on pipeline and pipeline,
Hypomere receiver (42) are made up of Pyrex material.
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| CN108926862A (en) * | 2018-09-29 | 2018-12-04 | 天津中福环保科技股份有限公司 | Light naphtha recyclable device, its skid structure and light naphtha recovery method in a kind of dangerous waste process field |
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| CN106433738B (en) | 2017-12-29 |
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