CN106556549B - A kind of method and apparatus of oil plant air-distillation column overhead scaling rate test - Google Patents
A kind of method and apparatus of oil plant air-distillation column overhead scaling rate test Download PDFInfo
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Abstract
The present invention relates to the test methods and device of a kind of oil plant air-distillation column overhead scaling rate, are followed successively by heating kettle, glass filler tower, tower head, air cooler from top to bottom；Pressure gauge, material inlet are provided on heating kettle；Tower head middle and upper part is provided with dirt pocket；Glass filler tower tower body draws a plurality of side line and picks up sample receiving flask respectively and control sampling quantity by shut-off valve；Injection port and thermocouple are provided on air cooler；Glass filler tower and tower head are equipped with insulating layer；Dirt pocket goes up position in being arranged in tower head, is made of cross hang, test piece, filler and bent fine grain pipe；Tower head section is arranged radially one perpendicular to axis and intersects at the cross hang of axis, supported and suspended scale collecting slot, filler is placed in scale collecting slot, scale collecting slot bottom is connected through a screw thread bent fine grain pipe.It is interior in tower reactor that material to be measured is added, dirt pocket then is installed in tower head middle and upper part detection zone.Invention becomes the intuitive effective means for calculating scaling rate, predicting the crude oil atmospheric distillation tower cycle of operation.
Description
Technical field
The invention belongs to the corrosion simulated fields of petrochemical industry atmospheric and vacuum distillation unit.
Background technique
Crude oil atmospheric vacuum distillation device is entire oil-refining chemical " faucet device ", and bearing is subsequent secondary operation device
The important task of raw material and product is provided, process procedure is very important.However for a long time, with crude oil heaviness, in poor quality
Trend it is increasingly apparent, the reasons such as auxiliary agent, air-distillation dress are used during electro-desalting scarce capacity and oil extraction in addition
The positions such as tower top heat exchanger and cooler salt crust is set to be on the rise.
It is sent to the crude oil of oil plant often saliferous band water from oil field, leads to the corrosion of equipment, in equipment inner wall fouling and shadow
Ring the composition of product oil.The corrosion at oil plant atmospheric distillation plant tower top low temperature position and dirty mineralization are to influence device long period
The principal element of safe operation.Ten million ton of oil refining apparatus of Plant of Tianjin Petrochemical Company is most of to process based on high-sulfur crude oil containing chlorine, atmospheric tower
Top circulation scale problems are always existed, the daily production run of device has been seriously affected.Atmospheric Tower recycles fouling, on the one hand reduces
Tower top conducts heat load, and then increases plant energy consumption；Another aspect foulant increasingly increases, if forming part obstruction, can make
At the unplanned parking of device；In addition, dirt is easily adhered in equipment, underdeposit corrosion is caused.It is reported that Urumchi petrochemical industry, the Yanshan Mountain
The generally existing such problems of the Petrochemical Enterprises such as petrochemical industry, Luoyang Petrochemical.
Fouling corrosion causes equipment installation surface appearance to deteriorate, energy consumption increases, and influences normally to produce, increases production cost,
Even cause to stop production.For a long time, refinery equipment safety and reliability are always to perplex the technical problem of its long-term operation.
For many years, numerous scholars' heat exchanging device fouling corrosion both domestic and external has carried out a large amount of research, but existing achievement only rests on
The level of qualitative research, such as fouling mechanisms, descaling method, the research for slowing down corrosion.Fouling in crude oil processing is not established
Quantitative appraisal index, i.e., to the measurement of practical scaling rate, there are no relevant reports.And the measurement of scaling rate can be more
The influence factor that oil product, temperature, water quality and injecting etc. generate dirty salt is intuitively understood, prediction crude oil atmospheric distillation tower fortune is become
The important intuitive means of one of row period.Patent CN203432891U simulates tower tray and filler corrosion in atmospheric and vacuum distillation unit
Experimental provision emphasis simulation destilling tower different location column plate and filler corrosion, do not consider fouling and fouling to corrosion
Influence；Therefore, crude oil processing average fouling rate evaluation method is established, the interaction of fouling and corrosion is grasped, comments
Valence oil product superiority and inferiority, desalting effect establish fouling evaluation system for oil refining plate and provide theoretical foundation, it appears particularly important, refinery
Enterprise has stepped an important step by four Nian Yixiu, five Nian Yixiu that march toward.
Summary of the invention
The object of the present invention is to provide the test methods of average structure rate in crude oil processing, intuitively observe fouling
With the generating process of corrosion, result can be used as the superiority and inferiority of evaluation oil product, the quality of desalting effect.
It is mounted on the dirt pocket simulation heat exchanger environment at tower head position, simulated normal pressure overhead mass transfer, exchange heat environment,
It can be intuitive to see the generating process of the heat exchanger salt crust in dew point.Built-in dirt pocket has horizontal and vertical flowing
Section, the withdrawing oil and injecting of tower top flow through strip, and by the capillary coiled pipe of dirt pocket, dirt is trapped.
Technical scheme is as follows:
A kind of device of oil plant air-distillation column overhead scaling rate test；Device be followed successively by from top to bottom heating kettle,
Glass filler tower, tower head, air cooler；Pressure gauge, material inlet are provided on heating kettle；Tower head middle and upper part is provided with dirt pocket；
Glass filler tower tower body draws a plurality of side line and picks up sample receiving flask respectively and control sampling quantity by shut-off valve；It is provided on air cooler
Injection port and thermocouple；Glass filler tower and tower head are equipped with insulating layer；Dirt pocket goes up position in being arranged in tower head, by cross
Support, test piece, filler and bent fine grain pipe composition；Tower head section is arranged radially one perpendicular to axis and intersects at the cross-shaped of axis
Support, supported and suspended scale collecting slot, scale collecting slot is interior to place filler, and scale collecting slot bottom is connected through a screw thread bent fine grain pipe.
The suspension wire is that it is overlapped with tower head axis, and liquid-phase reflux is enabled to cover entire test piece.
The test piece suspension wire is high temperature resistant, corrosion-resistant；Raschig ring stainless (steel) wire ring is loaded in dirty salt collector；Collector
For capillary coiled pipe, for retaining dirty salt.Carry out corrosion of the quantitative analysis crude oil to equipment by the weight change of the test piece
Effect；Scaling rate is quantitatively determined by the weight change of dirty salt collector.Raschig ring stainless steel be 10-30 block 2.5 ×
2.5mm Raschig ring stainless (steel) wire ring.
The method of oil plant air-distillation column overhead scaling rate test of the invention, the interior addition determinand in tower reactor
Then material installs dirt pocket in tower head middle and upper part detection zone, begin to warm up reflux operation after temperature is arranged.
The heating kettle volume 500-3000ml, 300 DEG C of heating kettle use temperature range >.
The glass filler tower internal diameter 30-50mm, height 1.0-2.0m；It is Raschig ring ceramic ring that material is loaded in it；Side line 3
A sample tap, sample tap can simultaneously thermometric；Two sections king-post sets independent heat preservation.Raschig ring ceramic ring is 2.0 × 2.0mm.
Suspension wire of the invention is overlapped with tower head axis, and liquid-phase reflux is enabled to cover entire test piece.
Tower head is infinite reflux, and tower top, tower head, tower body upper, middle and lower set thermometric, open up a normally closed type in the middle part of aerial condenser
Injecting mouth, for injecting purified water, organic amine, corrosion inhibiter and dirt dispersion agent into tower.
Unit simulation air-distillation column overhead mass transfer described in invention, heat exchange environment, can be intuitive to see in dew point
The generating process of heat exchanger salt crust in range, and then will be seen that the influence that oil product, temperature, water quality and injecting etc. generate dirty salt
Factor becomes an intuitive effective means for calculating scaling rate, predicting the crude oil atmospheric distillation tower cycle of operation.
The innovation of the invention consists in that:
(1) it has been put forward for the first time the design method of crude oil scaling rate test device in process；
(2) simulated normal pressure overhead mass transfer, heat exchange environment, can be intuitive to see the heat exchanger knot in dew point
The generating process of salt；
(3) it can really reflect the practical fouling condition of heat exchanger tube pass, and then deduce the operation of atmospheric and vacuum distillation unit
Period.
Detailed description of the invention
Fig. 1 is air-distillation column overhead scaling rate test device schematic diagram；
Fig. 2 is the schematic diagram of dirt pocket；
In Fig. 1: 1-glass tower reactor；2-glass tower bodies；3-tower heads；4-air coolers；5-injecting mouths；6-dirt pockets；
7-sampling receiving flasks；8-pressure gauges；9-material inlets；10-cooling waters；TI-warm galvanic couple；TCL-temperature-control heat couple；
11-cross hang；12-test pieces；13-Raschig ring fillers；14- song fine grain pipe.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings: device described in this method as shown in Figure 1, 2
It is followed successively by heating kettle 1, glass filler tower 2, tower head 3, air cooler 4 from top to bottom；Pressure gauge 8 is provided on heating kettle, material enters
Mouth 9；3 middle and upper part of tower head is provided with dirt pocket 6；Glass filler tower tower body draws a plurality of side line and picks up sample receiving flask 7 respectively and pass through
Shut-off valve controls sampling quantity；Injection port 5 and thermocouple are provided on air cooler 4；Glass filler tower and tower head are equipped with insulating layer；Collection
Dirty device goes up position in being arranged in tower head, is the core part for simulating scaling rate, by cross hang 11, test piece 12, filler
13 form with bent fine grain pipe 14；Tower head section is arranged radially one perpendicular to axis and intersects at the cross hang 11 of axis, support
Scale collecting slot is hung, places filler 13 in scale collecting slot, scale collecting slot bottom is connected through a screw thread bent fine grain pipe 14.
System guarantees that each position of destilling tower is tightly connected before opening intact, and tower head middle and upper part disposes dirt pocket, guarantees suspension wire
It is overlapped with tower head axis.Filling Raschig ring ceramic ring and test piece lower part are in close contact in dirt pocket, guarantee test piece section utmostly mould
Quasi- heat exchanger internal corrosion salt crust situation.Lifting platform height is adjusted, contacts heating mantle and tower reactor good；By each section temperature control and survey
Warm galvanic couple is put into the hole of corresponding position, and top casing and tower reactor casing inject silicone oil, is plugged thermocouple temperature measurement point.It will divide
In condensate oil product injection heating kettle 1 (to kettle 2/3rds), lead to coolant liquid, open power supply, opens heating and heat preservation.Temperature tends to
After steady, start from tower top injecting entrance injection purified water, organic amine, corrosion inhibiter etc..The heated oil gas of crude oil rises in tower reactor,
Purified water, corrosion inhibiter, organic amine, dirt dispersion agent that entrained corrosive gas, steam etc. are injected with injection port etc. is in collection dirt
Test piece is corroded in the simulation cold exchange device environment formed in device and generates fouling.Continuous operation for a period of time after, capillary
Coiled pipe blockage phenomenon.Stop heating, cooling down.It is careful to take out lacing film and dirt pocket, it weighs respectively.
The formula of scaling rate, corrosion rate and line clogging time is as follows:
vFouling=(w1-w0)/t (1)
vCorrosion=(h1-h0)/t (2)
TBlocking=VPipe×ρ/vFouling (3)
Wherein vFoulingIt is simulation scaling rate g/d；w0It is dirt pocket original weight g；w1It is dirt pocket weight g after simulating fouling；T simulation
Device runing time d；vCorrosionIt is lacing film corrosion rate g/d；TBlockingIt is the time d for predicting heat exchanger and blocking；h1It is lacing film corruption
Weight g before erosion；h0It is the weight g after lacing film corrosion；VPipeIt is the volume of heat exchanger tube pass 100mm；The density g/cm of ρ fouling3。
The operating parameter includes that overhead reflux is infinite reflux, and a normally closed type injection is opened up in the middle part of aerial condenser
Mouthful, the injection port is used to inject purified water, organic amine, corrosion inhibiter, dirt dispersion agent into tower.
The system temperature includes one 80-120 DEG C of line temperature of side, 100-140 DEG C of temperature of side two wires, three line temperature of side
120-160 DEG C, four 150-190 DEG C of line temperature of side, column pressure difference 0-10mm water column；The heating kettle volume 500-3000ml, adds
100-500 DEG C of hot jacket use temperature range.
Glass filler tower rectifying the column internal diameter 30-50mm, height 1.0-2.0m；It is Raschig ring that material is loaded in it
2.0 × 2.0mm ceramic ring；Number of theoretical plate 10-20 block, 3 sample taps of side line, sample tap can simultaneously thermometric；Two sections king-post is set
Independent heat preservation.
The tower head is used to simulate oil plant atmospheric distillation tower overhead condenser heat exchange environment, and tower head section radially opens up one
Perpendicular to axis and the cross hang of axis is intersected at, test piece is hung under the action of suspension wire, dirty salt collector is arranged in lower section.
The suspension wire is that it is overlapped with tower head axis, and liquid-phase reflux is enabled to cover entire test piece.
The test piece suspension wire is high temperature resistant, corrosion-resistant；10-30 block 2.5 × 2.5mm Raschig ring is loaded in dirty salt collector
(stainless steel)；Collector is capillary coiled pipe, for retaining dirty salt.Carry out quantitative analysis original by the weight change of the test piece
Corrosive effect of the oil to equipment；Scaling rate is quantitatively determined by the weight change of dirty salt collector.
Embodiment 1
By taking Saudi Arabia light oil as an example, density (20 DEG C) 857.5kg/m3, salt content 7.52mg/kg, chlorinity
5.52mg/kg, sulfur content 1.834%, acid value 0.0374mgKOH/g, viscosity (50 DEG C) mm2/s.Claim lacing film A weight 11.4613g,
Dirt pocket (containing magnet ring) weight 15.8372g.Interior addition 350ml crude oil to be measured in 500ml tower reactor is taken, while several ceramic rings are added,
To prevent bumping, test piece section disposes dirt pocket, guarantees that suspension wire is overlapped with test piece section axis, liquid-phase reflux is enabled to cover entire examination
Piece.10 Raschig ring stainless steels of filling and test piece lower part are in close contact in dirt pocket, guarantee that test piece section utmostly simulates heat exchange
Device internal corrosion salt crust situation.
Select 30mm internal diameter, the glass tower body of normal 1m fills each interface after tower in tower, smears vacuum grease, and small
The heart is installed together；When tower head connects, gasket is put well, to screw thread pressure-pad just, is carefully tightened, guarantee that tower body is vertical；It adjusts and rises
Platform height is dropped, contacts heating mantle and tower reactor good；Each section temperature control and temperature thermocouple are put into the hole of corresponding position, pushed up
Parts casing pipe and tower reactor casing inject silicone oil, are plugged thermocouple temperature measurement point；Logical coolant liquid opens power supply, heating and heat preservation such as table 1.
After temperature tends to be steady, as shown in table 1, start from tower top injecting entrance injection purified water, organic amine, corrosion inhibiter
Deng.After running 480h, capillary coiled pipe blockage phenomenon.Stop heating, cooling down.It is careful to take out lacing film A and dirt pocket,
Weigh 11.0560g, 20.8024g respectively.
According to oil plant atmospheric distillation plant E107 heat exchanger tube pass internal diameter 20mm, length 100mm is taken, the section is calculated
Shell side volume 3.14 × 10-5m3, the density of dirty sample is 1.5825g/cm3, the Saudi Arabia light oil can be calculated to test piece
Corrosion rate be 0.0203g/d, scaling rate 0.2483g/d, prediction heat exchanger tube pass is blocked by 200 day time.
1 temperature controlling range of table
Embodiment 2
By taking Saudi Arabia light oil as an example, density (20 DEG C) 857.5kg/m3, salt content 7.52mg/kg, chlorinity
5.52mg/kg, sulfur content 1.834%, acid value 0.0374mgKOH/g, viscosity (50 DEG C) mm2/s。
Lacing film B is claimed to weigh 11.5766, dirt pocket (containing magnet ring) weight 15.3857g.Take interior addition 1300ml in 1500ml tower reactor
Crude oil to be measured, while several ceramic rings are added, to prevent bumping, test piece section disposes dirt pocket, guarantees suspension wire and test piece section axis weight
It closes, liquid-phase reflux is enabled to cover entire test piece.20 Raschig ring stainless steels of filling closely connect with test piece lower part in dirt pocket
Touching guarantees that test piece section utmostly simulates heat exchanger internal corrosion salt crust situation.
Select 40mm internal diameter, the glass tower body of normal 1.5m, fill tower after tower each interface, smear vacuum grease, and
Careful is installed together；When tower head connects, gasket is put well, to screw thread pressure-pad just, is carefully tightened, guarantee that tower body is vertical；It adjusts
Lifting platform height contacts heating mantle and tower reactor good；Each section temperature control and temperature thermocouple are put into the hole of corresponding position,
Top casing and tower reactor casing inject silicone oil, are plugged thermocouple temperature measurement point；Logical coolant liquid opens power supply, heating and heat preservation such as table
2。
After temperature tends to be steady, as shown in table 1, start from tower top injecting entrance injection purified water, organic amine, corrosion inhibiter
Deng.After running 450h, capillary coiled pipe blockage phenomenon.Stop heating, cooling down.It is careful to take out lacing film A and dirt pocket,
Weigh 10.7041g, 20.4861g respectively.The Saudi Arabia light oil can be calculated is to the corrosion rate of test piece
0.0465g/d, scaling rate 0.2720g/d, prediction heat exchanger tube pass were blocked by 183d days time.
2 temperature controlling range of table
Embodiment 3
By taking Saudi Arabia light oil as an example, density (20 DEG C) 857.5kg/m3, salt content 7.52mg/kg, chlorinity
5.52mg/kg, sulfur content 1.834%, acid value 0.0374mgKOH/g, viscosity (50 DEG C) mm2/s。
Claim lacing film C weight 11.6198g, dirt pocket (containing magnet ring) weight 15.3857g.Take interior addition 2500ml in 3000ml tower reactor
Crude oil to be measured, while several ceramic rings are added, to prevent bumping, test piece section disposes dirt pocket, guarantees suspension wire and test piece section axis weight
It closes, liquid-phase reflux is enabled to cover entire test piece.30 Raschig ring stainless steels of filling closely connect with test piece lower part in dirt pocket
Touching guarantees that test piece section utmostly simulates heat exchanger internal corrosion salt crust situation.
Select 50mm internal diameter, the glass tower body of normal 2.0m, fill tower after tower each interface, smear vacuum grease, and
Careful is installed together；When tower head connects, gasket is put well, to screw thread pressure-pad just, is carefully tightened, guarantee that tower body is vertical；It adjusts
Lifting platform height contacts heating mantle and tower reactor good；Each section temperature control and temperature thermocouple are put into the hole of corresponding position,
Top casing and tower reactor casing inject silicone oil, are plugged thermocouple temperature measurement point；Logical coolant liquid opens power supply, heating and heat preservation such as table
3。
After temperature tends to be steady, as shown in table 1, start from tower top injecting entrance injection purified water, organic amine, corrosion inhibiter
Deng.After running 500h, capillary coiled pipe blockage phenomenon.Stop heating, cooling down.It is careful to take out lacing film C and dirt pocket,
Weigh 10.7139g, 20.8274g respectively.The Saudi Arabia light oil can be calculated is to the corrosion rate of test piece
0.04348g/d, scaling rate 0.2612g/d, prediction heat exchanger tube pass were blocked by 190.2d days time.
3 temperature controlling range of table
Heat exchanging device in embodiment is consistent with the runing time in the practical distillation process of crude oil using the predicted value of time,
The unit simulation can simulated normal pressure overhead mass transfer, heat exchange environment very well, can be intuitive to see in dew point model
The generating process for enclosing interior heat exchanger salt crust, objectively and accurately investigated influence that temperature, water quality and injecting etc. generate dirty salt because
Element.
Claims (9)
1. a kind of device of oil plant air-distillation column overhead scaling rate test, adds it is characterized in that device is followed successively by from top to bottom
Hot kettle, glass filler tower, tower head, air cooler；Pressure gauge, material inlet are provided on heating kettle；Tower head middle and upper part is provided with collection
Dirty device；Glass filler tower tower body draws a plurality of side line and picks up sample receiving flask respectively, and controls sampling quantity by shut-off valve；Air cooler
Upper setting injection port and thermocouple；Glass filler tower and tower head are equipped with insulating layer；Dirt pocket goes up position in being arranged in tower head,
It is made of cross hang, test piece, filler and bent fine grain pipe；Tower head section is arranged radially one perpendicular to axis and intersects at axis
Cross hang, supported and suspended scale collecting slot, scale collecting slot is interior to place filler, and scale collecting slot bottom is connected through a screw thread bent fine grain pipe.
2. device as described in claim 1, it is characterized in that the vertical line of test piece is overlapped with tower head axis, enable liquid-phase reflux
Cover entire test piece.
3. device as described in claim 1, it is characterized in that loading stainless steel Raschig ring in the dirt pocket；Bent fine grain pipe is
Capillary coiled pipe.
4. device as claimed in claim 3, it is characterized in that the stainless steel Raschig ring is 2.5 × 2.5mm of 10-30 block.
5. device as described in claim 1, it is characterized in that glass filler tower the internal diameter 30-50mm, height 1.0-2.0m；
It is ceramic ring Raschig ring that material is loaded in it；3 sample taps of side line, sample tap can simultaneously thermometric；Two sections king-post sets independent guarantor
Temperature.
6. device as claimed in claim 5, it is characterized in that the ceramic ring Raschig ring is 2.0 × 2.0mm.
7. such as device according to any one of claims 1 to 6, it is characterized in that the heating kettle volume 500-3000ml, adds
Hot kettle uses 300 DEG C of temperature >.
8., it is characterized in that tower head is infinite reflux, opening up one in the middle part of air cooler such as device according to any one of claims 1 to 6
A normally closed type injecting mouth, for injecting purified water, organic amine, corrosion inhibiter, dirt dispersion agent into tower.
9. the method for device to test scaling rate described according to claim 1~any one of 6, it is characterized in that adding in tower reactor
Enter material to be measured, dirt pocket then is installed in tower head middle and upper part detection zone, begins to warm up reflux operation after temperature is set；According to
Corrosive effect of the weight change quantitative analysis crude oil of test piece to equipment；Fouling is quantitatively determined according to the weight change of dirt pocket
Rate.
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| CN110487710A (en) * | 2019-09-12 | 2019-11-22 | 北京赛福贝特能源技术服务有限公司 | A kind of visualization device of crude(oil)unit overhead system fouling corrosion |
| FR3108415B1 (en) * | 2020-03-18 | 2022-04-01 | Total Sa | Method for predicting clogging of distillation column(s) of a refinery, computer program and associated prediction system |
| CN112345437A (en) * | 2020-10-28 | 2021-02-09 | 中国石油化工股份有限公司 | Method and device for evaluating corrosion inhibitor on atmospheric tower top of atmospheric and vacuum distillation unit |
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| CN106556549A (en) | 2017-04-05 |
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