CN110196302A - Automatic flushing device used in a kind of column chromatography adsorbing separation - Google Patents
Automatic flushing device used in a kind of column chromatography adsorbing separation Download PDFInfo
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- CN110196302A CN110196302A CN201810162083.2A CN201810162083A CN110196302A CN 110196302 A CN110196302 A CN 110196302A CN 201810162083 A CN201810162083 A CN 201810162083A CN 110196302 A CN110196302 A CN 110196302A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/38—Flow patterns
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Abstract
Automatic flushing device used in a kind of column chromatography adsorbing separation, including chromatographic column (10), sampling system and rinse-system, the sampling system includes sample introduction cup (2) and the switch valve (8) on the suction line on sample introduction cup cup lid, rinse-system includes peristaltic pump (3) and coupled multiposition valve (9) and the solvent bottle (1) that is connected with multiposition valve difference entrance, the sampling system is connect with rinse-system by triple valve (4), one end of triple valve is connect with chromatographic column column joint (12), in addition both ends are connected with the outlet end of the outlet end of peristaltic pump and sample introduction cup respectively, one entrance of the multiposition valve is connected with compressed-air line, compressed-air line is also connected with the switch valve on the suction line on sample introduction cup cup lid.The device can carry out automatic switchover flushing to the chromatographic column for having adsorbed tested oil sample with different rinse solvents, to separate different components.
Description
Technical field
The present invention relates to a kind of column chromatography adsorbing separation flushers, specifically, being a kind of for heavy oil separation hydrocarbon system
The column chromatography adsorbing separation automatic flushing device of component.
Background technique
Hydrocarbon system's composition is the elementary item of heavy oil property analysis, to instructing research and production to be of great significance.Currently, column
Chromatography adsorption separation method is still the most basic separation method of petrochemical field, is widely used in four component analysis of residual oil, lubricating oil
Potential content, four component analysis of pitch and crude oil wax content analysis etc..Heavy oil enters column chromatography with solvent during the separation process, by
Absorption of the different component in column chromatography stationary phase and analytic ability difference in heavy oil, thus can be incited somebody to action by adsorption capacity difference
Heavy oil is divided into different component.Its separating effect factors such as strong and weak, eluant, eluent type and dosage, eluant, eluent flow velocity by stationary phase polarity
It influences.Traditional pillar layer separation experiment is all full manual operations, there are complex steps, analytical cycle is long, data redundancy and
The problems such as accuracy is poor, consumption of organic solvent is big, big to the harm of operator's health.
CN102527088B discloses a kind of four component separating device of pressure-reducing type asphalt, by the way that vacuum pump control system is arranged
The flow velocity of flushing liquor is controlled, but irrigation used in the adsorbent different component of flushing and receiving bottle still need to replace manually,
Can only realize semi-automation flushing.
CN204241297U discloses a kind of four component separating device of pitch, and vacuum pump control system is installed on probe tube
It is rinsed on the device of flow velocity with controlling, by the way that probe tube is arranged between chromatographic column and flushing liquor receiving bottle, passes through sampling analysis
It determines whether there is aromatic hydrocarbons outflow in eluent, and replaces receiving bottle manually in aromatic hydrocarbons outflow.
Summary of the invention
The object of the present invention is to provide automatic flushing device used in a kind of column chromatography adsorbing separation, which can be with different
Rinse solvent carries out automatic switchover flushing to the chromatographic column for having adsorbed tested oil sample, to separate different components.
Automatic flushing device used in column chromatography adsorbing separation provided by the invention, including chromatographic column, sampling system and flushing
System, the sampling system include sample introduction cup and the switch valve on the suction line on sample introduction cup cup lid, rinse-system
Including peristaltic pump and coupled multiposition valve and the solvent bottle being connected with multiposition valve difference entrance, the sampling system with
Rinse-system is connected by triple valve, and one end of triple valve connect with chromatographic column column joint, in addition both ends respectively with peristaltic pump
Outlet end is connected with the outlet end of sample introduction cup, and an entrance of the multiposition valve is connected with compressed-air line, compressed air hose
Line is also connected with the switch valve on the suction line on sample introduction cup cup lid.
Chromatographic column is connect with sampling system and rinse-system by triple valve by the present invention, and rinse-system is connected by multiposition valve
The multiple solvent bottles of control are connect, so as to realize and adsorbed with different solvents auto-flushing chromatographic column by the entrance for changing multiposition valve
Component, separate oil sample in different component.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention.
Fig. 2 is the structural schematic diagram of sampling system in apparatus of the present invention.
Fig. 3 is the structural schematic diagram of automatic decanting device provided by the invention.
Specific embodiment
Column chromatography adsorbing separation automatic flushing device provided by the invention, by triple valve by sampling system and rinse-system
It is connected, oil sample solution can be pressed into chromatographic column by sampling system by compressed air, the controllable different flushing of rinse-system
Solvent constant speed quantitatively rinses chromatographic column, and the different component of absorption is rinsed, to realize point of different component in oil sample
From, in addition, automatic flushing device chromatographic column outflux lower part place automatic decanting device, can solvent switch when or setting it is stagnant
Automatically switch flushing liquor receiving bottle under flush volume afterwards, collects the different component isolated respectively.The device have it is easy to operate,
It is molten to significantly reduce flushing in addition, whole device carries out automatically in confined conditions for data redundancy and the high advantage of accuracy
Harm of the agent to operator's health.Compared to traditional manual analytical methods, apparatus of the present invention are rinsed and flushing liquor is collected
It realizes automation, and multiple samples can be separated simultaneously with multiple chromatographic columns side by side, share a set of rinse solvent system,
Substantially increase the efficiency of oil product different component separation analysis.
Sampling system of the present invention includes sample introduction cup and the switch valve on sample introduction cup cup lid upper inlet pipeline, is opened
It closes valve to be connected with compressed-air line, the sample introduction cup includes cup body and cup lid, and cup lid is equipped with suction line, sets on cup body
Outlet end.Preferably, a transparent sample introduction observation tube is set, between sample introduction cup and the connecting pin of triple valve to observe sample introduction
After the completion, triple valve is switched into flush position.The preferred electromagnetic switch valve of the switch valve.
Rinse-system of the present invention include peristaltic pump and coupled multiposition valve and with multiposition valve difference entrance
Connected solvent bottle.The multiposition valve is equipped with multiple entrances, can be communicated different entrances with outlet by switching, thus available
The solvent contained in different solvents bottle is rinsed chromatographic column.The multiposition valve is preferably provided with 4~12 entrances, therein
One entrance is connected with compressed-air line, remaining each entrance is connected with a solvent bottle, and the compressed air inlet is used
In being purged and dried with pipeline of the air to multiposition valve to chromatographic column after the completion of flushing.
The multiposition valve is preferably electronic multiposition valve, and can pass through the switching of each entrance of process control.
The peristaltic pump is preferably program-controlled peristaltic pump, and can be by process control and calibration flushing liquor irrigation flow rate, such as
This, passes through control time i.e. controllable rinse solvent dosage.
Preferably, the adsorption column is placed in chromatographic column temperature control box, and multiple colors can be arranged in parallel in the temperature control box
Column is composed, each chromatographic column passes through triple valve and sampling system is connected with rinse-system.It therefore, can be empty by sharing a set of compression
Gas admission line and flushing liquid supply system carry out sample introduction and flushing operation to each chromatographic column.
Automatic decanting device is placed in the chromatographic column bottom end, and automatic decanting device includes transmission parts and placed on it puts punching
The support plate of washing lotion receiving bottle, and make the flushing of the bottleneck of each flushing liquor receiving bottle face adsorption column bottom end at the appointed time
Liquid outlet.
Transmission parts in above-mentioned automatic decanting device are horizontally moveable, vertically move or moving in rotation.
Preferably, transmission parts described in the automatic decanting device include stepper motor and threaded rod connected to it, institute
State setting band movable slider on threaded rod, fixed support plate on band movable slider.Flushing liquor receiving bottle, stepper motor are placed in support plate
Threaded rod is driven to move horizontally, so that support plate be driven to move horizontally, the flushing liquor receiving bottle placed thereon is also horizontal therewith to be moved
It is dynamic.
Sampling system described in apparatus of the present invention, rinse-system, automatic decanting device, chromatographic column temperature control box can be by controlling automatically
System control processed, chromatographic column when including sample introduction operation moisten column, and the flushing liquor dosage of rinse-system, flushing speed, flushing liquor are cut
It changes, the flushing liquor receiving bottle switching in automatic decanting device, i.e., available single-chip microcontroller or computer work control each entrance of multiposition valve are cut
It changing the time, peristaltic pump is pumped into flushing liquor speed and time, and automatic decanting device corresponds to the mobile transmission parts of different flushing liquor collecting amounts,
After flushing liquor needed for making a kind of separation component rinses, the punching of subsequent rinse liquid is received with another empty flushing liquor receiving bottle
The separation component to get off is washed, and so on, until flushing out all required different separation components with different flushing liquors.Institute
The same separation component stated can be rinsed with different flushing liquors, can be put into separation component in one flushing liquor receiving bottle, because
This, n flushing liquor receiving bottle of n separation component, the last one flushing liquor receiving bottle is produced for reception air blow line
Raw waste liquid.
Automatic flushing device used in column chromatography adsorbing separation provided by the invention can be used for residual oil, lube base oil,
The separation of the saturated hydrocarbons, aromatic hydrocarbons and glial component of the heavy oil such as pitch and crude oil.Have the advantages that automatic, efficient, repeated good.
The present invention is further illustrated with reference to the accompanying drawing.
Fig. 1 is schematic structural diagram of the device of the invention, and wherein the lower end of triple valve 4 is connect with the column joint of chromatographic column 10,
Horizontal both ends, one end are connected by pipeline with the outlet line of 2 cup body of sample introduction cup, and the other end passes through pipeline and peristaltic pump 3
Outlet is connected, and electromagnetic switch valve 8 is set on the suction line 21 on 2 cup lid of sample introduction cup, and be connected with compressed-air line, and compression is empty
Gas pipeline is equipped with pressure-regulating valve 7.The arrival end of the peristaltic pump is connected with the outlet end of multiposition valve 9.There are six multiposition valves
Entrance, one of entrance are connected with compressed-air line, and other each entrances are connected with a solvent bottle 1, the multiple molten
Solvent A, B, C, D, E are respectively provided in agent bottle.Column bottom is equipped with automatic decanting device 11, can place multiple flushing liquors thereon and connect
Receive bottle 6.The chromatographic column is placed in chromatographic column temperature control box 5.
Fig. 2 is the structural schematic diagram of sampling system in apparatus of the present invention, suction line 21 and electromagnetism on 2 cup lid of sample introduction cup
Switch valve 8 is connected, and the outlet end of 2 bottom of cup of sample introduction cup is equipped with sample introduction observation tube 22, the other end of sample introduction observation tube and threeway
The a port of valve is connected, another port of triple valve is connected with wriggling pump discharge 31, the lower port and chromatographic column of triple valve
10 column joint 12 connects.
Fig. 3 is a kind of structural schematic diagram of automatic decanting device provided by the invention, and threaded rod 17 is equipped with band movable slider 14,
One end is fixed, and the other end is connected with stepper motor 13, and a support plate 16 is fixed on band movable slider top, thereon placement tray
15, multiple flushing liquor receiving bottles are put in a row on pallet.When operation, stepper motor drives threaded rod rotation, band 14 He of movable slider
Support plate 16 makees horizontal rectilinear motion, to keep the flushing liquor receiving bottle horizontal linear being placed on stripe shape pallet mobile.With certainly
Autocontrol system controls stepper motor rotation and with movable slider timing movement, so that flushing liquor liquid collecting bottle is automatically moved switching, realizes
The automatic collection of separation component flushing liquor.
The operation of sample introduction process is as follows: triple valve 4 being placed in off, compressed air is adjusted to via pressure-regulating valve 7
Authorized pressure.Sample solution is poured into sample introduction cup 2, covers cup lid, swivel tee valve 4 to sample introduction state (sample introduction cup and chromatographic column
Connect), electromagnetic switch valve 8 is opened, sample solution is pressed into chromatographic column by air.Sample introduction observation tube 22 is observed, when sample solution end
After end enters chromatographic column by observation tube, triple valve is placed in off, sample introduction operation is completed.
The operation of sample wash process is as follows: by the setting of chromatographic column temperature control box 5 to required temperature, by flushing liquor liquid collecting bottle by volume
Number sequence is put well, and triple valve is placed in flushing state (peristaltic pump and chromatographic column are connected), by each entrance of multiposition valve by setting in advance
Fixed flushing liquor sets the flow value of peristaltic pump, flushing liquor is i.e. by compacted using required solvent bottle is sequentially successively switched on
It is dynamic to be pumped into chromatographic column, chromatographic column is rinsed, flushing liquor is to flow into the flushing liquor receiving bottle below chromatographic column, has been rinsed
Bi Hou, multiposition valve automatically switch entrance, are rinsed with next flushing liquor to chromatographic column, after being rinsed to a kind of component,
Automatic decanting device automatically moves, and next empty flushing liquor receiving bottle is moved to below chromatographic column, and so on, until flushing
Component separately flows into the washing lotion receiving bottle of setting.Last multiposition valve automatically switches to compressed air inlet, will remain in system
Rinse solvent cement out and drying system, in case test next time.
Before sample introduction, it is preferable that profit column is first carried out to chromatographic column using solvent, profit column solvent for use generally with rinse first
The solvent of a separation component is identical, therefore can place it in a flushing liquor receiving bottle.
Further illustrate the application method and separating effect of apparatus of the present invention below by example, but the present invention is not limited to
This.
Example 1
A residual oil sample is automatically analyzed with apparatus of the present invention.
(1) prepare stationary phase used in chromatographic column
The activation of aluminium oxide: it by neutral alumina in 500 DEG C of roasting 6h, is fitted into narrow-mouthed bottle after taking out cooling, by oxidation
Aluminum amount 1% be added distilled water, placed after acutely shaking up seal for 24 hours it is spare.
0.5860g residual oil sample is weighed with beaker, 10mL normal heptane is added and dissolves by heating, it is spare.
(2) cleaning procedure is set
Open automatic flushing device power supply of the present invention, start computer, open control program, be respectively set profit column program with
The parameter of cleaning procedure, irrigation flow velocity are controlled by peristaltic pump, and irrigation switching is controlled by multiposition valve, the switching of flushing liquor receiving bottle
It is controlled by automatic decanting device.Chromatograph box temperature control system is opened, by temperature setting at 50 DEG C.The flushing liquor receiving bottle weighed is pressed
Number is placed in automatic decanting device pallet.Profit column program and the parameter of cleaning procedure are shown in Tables 1 and 2 respectively.
Table 1
Table 2
(3) separation sample component is rinsed
Chromatographic column loads activated aluminium oxide and ram-jolt, is installed in temperature control box, and the port of column cap and triple valve is connected
It connects.Triple valve is placed in flushing state (peristaltic pump and chromatographic column connect), starting profit column program, the irrigation volume used in the profit column
When reaching setting value, flushing is automatically stopped.
The residual oil sample solution dissolved with normal heptane is poured into sample introduction cup, then latter with about 5mL normal heptane flushing beaker
And pour into, cup lid is covered, the entrance pressure that compressed air is adjusted with pressure-regulating valve is 40kPa (gauge pressure).Column program to be moistened is complete
Triple valve is placed in sample introduction state (sample introduction cup and chromatographic column are connected) by Cheng Hou, and solenoid valve is opened immediately, and sample solution is pressed into color
It composes in column.When observing that sample solution fully enters chromatographic column from sample introduction observation tube, triple valve is placed in off immediately.
Triple valve is placed in flushing state, while starting sample wash program, the rinse solvent described in table 2 rinses in order
Chromatographic column, after a kind of every flushing with rinse solvent, multiposition valve is automatically switched valve inlet and has been rinsed using next rinse solvent
After a kind of component, automatic decanting device is moved horizontally, and next flushing liquor receiving bottle is placed under chromatographic column automatically, to all flushings
After solvent is finished, the entrance of multiposition valve automatically switches to compressed-air line, remaining rinse solvent and does in exchange system
Drying system, cleaning procedure are completed.
Solvent in the separation component solution of collection is volatilized completely, then cooling, weighing calculates each component content
(mass fraction) are as follows: saturated hydrocarbons 45.2%, aromatic hydrocarbons 35.7%, (colloid+pitch) 16.6%.According to SH/T 0266-1992 petroleum
It is 2.4 mass % that asphalt content measuring method, which measures sample studies on asphaltene content, and calculating gum level is 14.2 mass %.
Example 2
A wax oil sample is automatically analyzed with apparatus of the present invention.
(1) prepare stationary phase used in chromatographic column
The activation of Kiselgel A: Kiselgel A is placed in culture dish, and in 175 DEG C of dry 3h, taking-up is put into drier
Be cooled to room temperature, be fitted into narrow-mouthed bottle seal it is spare.
0.9784g wax oil sample is accurately weighed with beaker, it is standby that 10mL petroleum ether (boiling range is 60 DEG C~90 DEG C) dissolution is added
With.
(2) cleaning procedure is set
Open automatic flushing device power supply of the present invention, start computer, open control program, be respectively set profit column program with
The parameter of cleaning procedure, rinse solvent flow velocity are controlled by peristaltic pump, and rinse solvent switching is controlled by multiposition valve, flushing liquor receiving bottle
Switching is controlled by automatic decanting device.Chromatograph box temperature control system is opened, by temperature setting at 50 DEG C.The flushing liquor weighed receives
Bottle is placed in by number in automatic decanting device pallet.The setup parameter of profit column program and cleaning procedure is shown in Table 3 and table 4 respectively.
Table 3
Table 4
(3) separation sample component is rinsed
Chromatographic column loads activated Kiselgel A and ram-jolt, is installed in temperature control box, by the port of column cap and triple valve
Connection.Triple valve is placed in flushing state (peristaltic pump and chromatographic column connect), starting profit column program, the irrigation body used in the profit column
When product reaches setting value, flushing is automatically stopped.
Sample introduction cup will be poured into the good wax oil sample solution of petroleum ether dissolution, then latter with about 5mL petroleum ether flushing beaker
And pour into, cup lid is covered, the entrance pressure that compressed air is adjusted with pressure-regulating valve is 25kPa (gauge pressure).Column program to be moistened is complete
Triple valve is placed in sample introduction state (sample introduction cup and chromatographic column are connected) by Cheng Hou, and solenoid valve is opened immediately, and sample solution is pressed into color
It composes in column.When observing that sample solution fully enters chromatographic column from sample introduction observation tube, triple valve is placed in off immediately.
Triple valve is placed in flushing state, while starting sample wash program, the rinse solvent described in table 4 rinses in order
Chromatographic column, after a kind of every flushing with rinse solvent, multiposition valve is automatically switched valve inlet and has been rinsed using next rinse solvent
After a kind of component, automatic decanting device is moved horizontally, and next flushing liquor receiving bottle is placed under chromatographic column automatically, to all flushings
After solvent is finished, the entrance of multiposition valve is switched into compressed-air line, remaining rinse solvent and drying in exchange system
System, cleaning procedure are completed.
Solvent in the separation component solution of collection is volatilized completely, then cooling, weighing calculates the content of each component
For (mass fraction): saturated hydrocarbons 68.6%, aromatic hydrocarbons 26.9%, colloid 4.5%.
Claims (9)
1. automatic flushing device used in a kind of column chromatography adsorbing separation, including chromatographic column (10), sampling system and rinse-system, institute
The sampling system stated includes sample introduction cup (2) and the switch valve (8) on the suction line on sample introduction cup cup lid, rinse-system packet
The solvent bottle (1) for including peristaltic pump (3) and coupled multiposition valve (9) and being connected with multiposition valve difference entrance, it is described into
Sample system is connect with rinse-system by triple valve (4), and one end of triple valve is connect with chromatographic column column joint (12), in addition both ends
It is connected respectively with the outlet end of the outlet end of peristaltic pump and sample introduction cup, an entrance and the compressed-air line phase of the multiposition valve
Even, compressed-air line is also connected with the switch valve on the suction line on sample introduction cup cup lid.
2. automatic flushing device described in accordance with the claim 1, it is characterised in that the multiposition valve is equipped with 4~12 entrances,
One of entrance is connected with compressed-air line, remaining each entrance is connected with a solvent bottle.
3. automatic flushing device described in accordance with the claim 1, it is characterised in that the multiposition valve is electronic multiposition valve, and can
Pass through the switching of each entrance of process control.
4. automatic flushing device described in accordance with the claim 1, it is characterised in that the switch valve (8) is electromagnetic switch valve.
5. automatic flushing device described in accordance with the claim 1, it is characterised in that the sample introduction cup of sampling system and the company of triple valve
It connects and sets a transparent sample introduction observation tube (22) between end.
6. automatic flushing device described in accordance with the claim 1, it is characterised in that the chromatographic column (10) is placed in chromatographic column temperature
It controls in case (5).
7. automatic flushing device described in accordance with the claim 1, it is characterised in that place automatic decanting in the chromatographic column bottom end
Device (11), automatic decanting device includes transmission parts and the support plate placed on it for putting flushing liquor receiving bottle (6), and makes each punching
The flushing liquor outlet of the bottleneck of washing lotion receiving bottle face chromatographic column bottom end at the appointed time.
8. automatic flushing device according to claim 7, it is characterised in that the transmission parts in automatic decanting device can be horizontal
It is mobile, vertically move or moving in rotation.
9. automatic flushing device according to claim 7, it is characterised in that the transmission parts packet of the automatic decanting device
Include stepper motor (13) and threaded rod connected to it (17), setting band movable slider (14) on the threaded rod, on movable slider
Fixed support plate (16).
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CN201810162083.2A CN110196302A (en) | 2018-02-27 | 2018-02-27 | Automatic flushing device used in a kind of column chromatography adsorbing separation |
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CN201810162083.2A CN110196302A (en) | 2018-02-27 | 2018-02-27 | Automatic flushing device used in a kind of column chromatography adsorbing separation |
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Citations (5)
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CN103323560A (en) * | 2012-03-23 | 2013-09-25 | 北京神州卓越石油科技有限公司 | Component separating preparation instrument |
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CN104730175A (en) * | 2015-04-10 | 2015-06-24 | 大连工业大学 | Automatic vacuum liquid-chromatography separator and control method thereof |
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2018
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CN2227338Y (en) * | 1995-03-28 | 1996-05-15 | 中国石油化工总公司石油化工科学研究院 | Liquid chromatography device for separating dead oil component |
US20110100146A1 (en) * | 2009-10-29 | 2011-05-05 | Hong Fu Jin Precision Industry (Shenzhen) Co., Ltd. | Robot arm |
CN103323560A (en) * | 2012-03-23 | 2013-09-25 | 北京神州卓越石油科技有限公司 | Component separating preparation instrument |
CN104655768A (en) * | 2015-03-11 | 2015-05-27 | 天津博纳艾杰尔科技有限公司 | Automatic crude oil component separating device and application of automatic crude oil component separating device in separation wax and colloid in crude oil |
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Application publication date: 20190903 |