CN105277482B - A kind of distilling apparatus overhead system dew point corrosion test method - Google Patents
A kind of distilling apparatus overhead system dew point corrosion test method Download PDFInfo
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Abstract
The invention discloses a kind of distilling apparatus overhead system dew point corrosion test methods.Its method is:1) processing work electrode and corrosion coupon;2) etchant solution pours into five mouthfuls of flasks, and Section II three-electrode system is fixed in three mouths of five mouthfuls of flasks, and five mouthfuls of flasks are fixed in digital display oil bath pan;3) other two mouth of five mouthfuls of flasks connects the horizontal inner tube inlet and outlet of condenser pipe respectively, and corrosion coupon is fixed in the horizontal inner tube of condenser pipe, and I three-electrode system is fixed on condenser pipe inclined tube top;4) five mouthfuls of flasks are heated with digital display oil bath pan, open I section condenser pipe outer tube cooling water inlet and Section II section condenser pipe outer tube cooling water inlet, cooling water flow is adjusted, carries out the electro-chemical test under acidic aqueous solution, the electro-chemical test experiment under the corrosion weight loss experiment and moisture condensation environment under moisture condensation environment later.The method of the present invention can carry out electro-chemical test but also carry out the dew point corrosion test of corrosion weight loss, realize the tests such as electrochemical impedance spectroscopy, electrochemistry noise of the material under dew point environment, the reliability of data can be verified again by weightless test.
Description
Technical field
The present invention designs a kind of distilling apparatus overhead system dew point corrosion test method and device, more particularly to
To a kind of method and device for the distilling apparatus overhead system dew point corrosion test that can realize electro-chemical test and corrosion weight loss.
Background technology
Dew point corrosion is a kind of corrosion phenomenon for being cooled to liquid by saturated vapor and causing to corrode to material.Distilling apparatus
The first coagulation zone for being happened at tower top and condensing cooling system of tower top dew point corrosion or the region there are partial condensation, in tower top oil gas
Most HCl enters in initial stage condensed water, and the concentration for forming hydrochloric acid solution may be up to 1~2wt%, makes dew point position condensed water
PH value it is very low, form very strong " the hcl corrosion environment " of a corrosivity.The HCl that ordinary decompression column top system occurs comes from crude oil
The hydrolysis of middle chloride.Chloride can be divided into two class of inorganic chlorine and organochlorine in crude oil.Inorganic villaumite mainly has NaCl, MgCl2
And CaCl2, the hydrolysis temperature and degree of three kinds of inorganic salts be different.At 350 DEG C, MgCl2And CaCl2Percent hydrolysis difference
It is 95% and 10% or so;NaCl only about 2% decomposes.
At the dew point position of overhead system, neutralizer NH3Water is not readily dissolved in, therefore does not have shadow to the pH value at dew point position
It rings, does not have neutralization.With the reduction of system temperature, the amount of condensed water is continuously increased, be constantly diluted due to HCl and
NH3The increase of meltage increases the pH value of water phase.The pH value of condensed water can not reflect in Atmospheric vacuum tower top gun barrel
The pH value situation of entire overhead system condensed water, this is also the original that dew point corrosion is known as the corrosion of distilling apparatus overhead system most serious
Cause.Dew point corrosion situation by condensate liquid chlorine ion concentration, pH value, oxygen content, environment temperature and equipment steel corrosion resistant
The influence of corrosion, therefore the dew point corrosion of the condensate cooler in atmospheric unit tower top is complicated, so the shape to dew point corrosion
Into and monitoring propose high requirement.
At present, what the domestic dew point corrosion behavior for material was reported is less.Patent CN101251467A and
CN101876622A describes a kind of evaluation material sulfur resistive acid dew piont corrosion respectively using sulfur dioxide and sulfur trioxide as medium
Test device and its test method that can be good and bad, be evaluated, the corrosive environment and reality of simulation by being weight-loss method
Dew point corrosion environment is closer to, and shortcoming is cannot to carry out the electrochemistry such as electrochemical impedance spectroscopy, electrochemistry noise in the present context
Test, means are single, are unfavorable for dew point corrosion mechanism study.Patent CN101929945A describes phosphorus pair in a kind of yellow phosphoric tail gas
The low-temperature dew point corrosion experimental method and device of boiler material, the invention by material different temperatures various concentration phosphoric acid solution
In invade bubble certain time, the dew point corrosion performance of material, corrosive environment are evaluated impregnating front and rear weight change by material
Deviate practical dew point corrosion environment, have ignored the condensation of acid, come off and the practical dew point corrosion environment such as the diffusion of coagulation,
The data obtained reliability is still to be tested.A kind of dew point corrosion that can realize electro-chemical test of patent CN102692438A inventions is real
Experiment device, but corrosion weight loss experiment cannot be carried out at the same time, the reliability of data cannot be verified by corrosion weight loss.
Invention content
The object of the present invention is to provide a kind of distilling apparatus overhead system dew point corrosion test method, this method can carry out
Electro-chemical test can carry out the dew point corrosion test of corrosion weight loss again, realize electrochemical impedance of the material under dew point environment
The tests such as spectrum, electrochemistry noise, the reliability of data can be verified again by weightless test.
The present invention provides a kind of distilling apparatus overhead system dew point corrosion test method, it is characterised in that including following steps
Suddenly:
1) preparation of two sets of electrochemical working electrodes:It will carry out the I working electrode of electro-chemical test and Section II work electricity
The cylinder of a diameter of 10~12mm is processed into pole respectively, and after applying envelope, solidification, polishing, polishing, oil removing and drying are spare;
The preparation of corrosion weight loss lacing film:The corrosion coupon for carrying out weightless test is processed into cuboid, is then polished step by step,
Oil removing, then move into absolute ethyl alcohol and impregnate 2~5 minutes, it takes out and dry, weighs after 24~48 hours for use;
2) etchant solution is poured into five mouthfuls of flasks, by prepared by Section II auxiliary electrode, step 1) Section II working electrode,
Section II reference electrode and thermometer are fixed in three mouths of five mouthfuls of flasks, immerse Section II auxiliary electrode and Section II reference electrode
Into etchant solution, Section II working electrode is totally submerged in etchant solution, and five mouthfuls of flasks then are fixed on digital display oil bath pan
In, Section II auxiliary electrode, Section II working electrode and Section II reference electrode are connected with electrochemical test, carry out acidic aqueous solution ring
Electro-chemical test under border;
3) other two mouth of five mouthfuls of flasks connects the horizontal inner tube import of condenser pipe and the horizontal inner tube outlet of condenser pipe respectively,
The horizontal internal tube of condenser pipe is provided with corrosion coupon stent, and the corrosion coupon prepared by step 1) is placed on corrosion coupon branch
It is fixed on frame, it is inserted into temperature in the input end of the horizontal inner tube of condenser pipe, the port of export and the thermometer socket of condenser pipe inclined tube lower part
Degree meter, the upper of condenser pipe inclined tube is fixed on by I working electrode, the I reference electrode prepared by I auxiliary electrode, step 1)
Portion carries out the electro-chemical test under moisture condensation environment with electrochemical test, then by the both ends of the horizontal inner tube of condenser pipe respectively with
Two mouths of five mouthfuls of flasks are connected, and fixed condenser pipe;
(4) dew-point temperature of etchant solution is calculated, digital display oil bath pan is opened and heats five mouthfuls of flasks, corrosive medium is made to boil,
Etchant gas and steam are generated, opens the cooling water inlet of I section condenser pipe outer tube and the cooling water of Section II section condenser pipe outer tube
Import, cooling water are entered by cooling water inlet, are flowed out from cooling water outlet, are adjusted the flow of cooling water, corrosive vapor is made to exist
Corrosion coupon and the condensation of I working electrode surface carry out the electro-chemical test under acidic aqueous solution, the corruption under moisture condensation environment at this time
Lose weightless test and the electro-chemical test experiment to condense under environment.
The present invention is further technically characterized in that:Prepared I working electrode and Section II work in the step 1)
Electrode is identical with the corrosion coupon material for carrying out corrosion weight loss experiment.
The present invention is further technically characterized in that:It is epoxy resin that material used in envelope is applied in the step 1), is removed
Oily material therefor is acetone.
The present invention is further technically characterized in that:Polishing described in the step 1) is to be polishing to 800 step by step with sand paper
~1200#.
Present invention employs two sets of electrochemical test systems, test respectively under acidic aqueous solution environment and moisture condensation environment
Electrochemical impedance spectroscopy and electrochemistry noise, so as to be confirmed under acidic aqueous solution environment and the moisture condensation environment of dew point corrosion with experiment,
The dew point corrosion mechanism of material is different, has further insight to dew point corrosion mechanism.
First set electrochemical test system in the present invention is used for testing the electrochemical impedance spectroscopy under acidic aqueous solution environment
And electrochemistry noise, including digital display oil bath pan, five mouthfuls of flasks, electrochemical test, thermometer and Section II three-electrode system.Section II
Three-electrode system, that is, Section II reference electrode, Section II auxiliary electrode and Section II working electrode, wherein Section II reference electrode can be Ag/
AgCl electrodes, Section II auxiliary electrode can be platinum electrode, and Section II working electrode is institute's test sample.
Second set of electrochemical test system in the present invention is used for testing the electro-chemical test under moisture condensation environment, including condensation
Pipe inclined tube, Section II section condenser pipe outer tube, thermometer, I three-electrode system and electrochemical test, I three-electrode system, that is, I
Reference electrode, I auxiliary electrode and I working electrode, wherein I reference electrode can be Ag/AgCl electrodes, I auxiliary electrode
Can be platinum electrode, I working electrode is institute's test sample.
Weightless test system in the present invention includes the horizontal inner tube of condenser pipe, I section condenser pipe outer tube, thermometer and corrosion
Lacing film.
The present invention experimental method be:
Five mouthfuls of flasks 2 for filling etchant solution are put into digital display oil bath pan 1, digital display oil bath pan heating corrosive medium,
It is allowed to boil, generates acid medium and steam.By Section II auxiliary electrode 3, Section II working electrode 4, Section II reference electrode 5, temperature
Meter 6 is fixed on rubber stopper in five mouthfuls of flasks, is allowed to be immersed in solution, Section II working electrode 4 will be totally submerged into corrosive liquid
In.The both ends of the horizontal inner tube 21 of condenser pipe are connected respectively with two mouths of five mouthfuls of flasks 2, realize the cycle of solution, ensure corrosion
The consistency of medium in the entire experiment process.By one group (6) parallel corrosion coupon 12, fixed, be placed on cold with test piece frame
In the horizontal inner tube 21 of solidifying pipe.Thermometer 10,11,13 is inserted into the input end of the horizontal inner tube 21 of condenser pipe, the port of export and cold respectively
In the thermometer socket of solidifying 14 lower part of inclined tube, to monitor the temperature of whole experiment process, determine to be carried out under conditions of dew point
Experiment.The cooling water of I section condenser pipe outer tube 7 and Section II section condenser pipe outer tube 20 enters respectively from mouth 8,15, from 9,16 streams
Go out, two-way cooling water can ensure that etchant gas total condensation is got off, and be allowed to flow back into five mouthfuls of flasks, and will be according to temperature
Meter adjusts the flow of cooling water, it is ensured that is carried out under the conditions of the tangible moisture condensation of experiment.Condensation inclined tube 14 another port top into
The another set of electrochemical test system of row, Section II auxiliary electrode 17, Section II working electrode 18, Section II reference electrode 19 is fixed on cold
The port of solidifying inclined tube 14, carries out the electro-chemical test under moisture condensation environment.
This experimental method is not limited solely to the research of distillation tower top hydrochloric acid dew point corrosion, can replace corrosion as needed
Medium, the dew point corrosion of the corrosive mediums such as research sulfuric acid, phosphoric acid.
The advantage of the invention is that:1. the corrosive environment that the present invention simulates is closer to practical dew point corrosion environment,
And electro-chemical test can be carried out.2. the present invention is provided with two sets of electrochemical test systems, acidic aqueous solution is tested respectively
Electrochemical impedance spectroscopy and electrochemistry noise under environment and moisture condensation environment can use experiment to confirm acidic aqueous solution environment and dew point
Under the moisture condensation environment of corrosion, the corrosion mechanism of material is likely to be different.3. the present invention is provided with corrosion weight loss and tests, electrification
Learning the result of test can be verified by weightless test.The present invention carries out under close dew temperature, normal pressure, easy to operate,
Safety is higher, and realizes closed circulation, does not generate pollution.
The present invention is described in further detail with reference to the accompanying drawings and detailed description, but is not intended to limit the present invention's
Range.
Description of the drawings
Fig. 1 is a kind of distilling apparatus overhead system dew point corrosion test method flow diagram of the present invention.
Reference numeral is shown in figure:
1- digital display oil bath pans;Five mouthfuls of flasks of 2-;3- Section II auxiliary electrodes;4- Section II working electrodes;5- Section II reference electrodes;
6th, 10,11,13- thermometers;7- I section condenser pipe outer tubes;14- condenser pipe inclined tubes;8th, 15- cooling water inlets;9th, 16- cooling waters
Outlet;12- corrosion coupons, 17- I auxiliary electrodes;18- I working electrodes;19- I reference electrodes;20- Section II section condenser pipes
Outer tube;The horizontal inner tube of 21- condenser pipes;22nd, 23- electrochemical tests.
Specific embodiment
As shown in Figure 1, a kind of distilling apparatus overhead system dew point corrosion test method.Its step is:
(1) preparation of the working electrode of electro-chemical test:It will carry out the working electrode of electro-chemical test, i.e. I work electricity
Pole and Section II working electrode, are processed into the cylinder of a diameter of 10~12mm, are welded with welding rod, are then applied and sealed with epoxy resin,
After solidification, abrasive paper for metallograph is polishing to 800~1200# step by step, is then polished, acetone oil removing, is wiped with absolute alcohol cotton balls,
Hair dryer dries up, and is put into spare in drying box;
The preparation of corrosion weight loss lacing film:The corrosion coupon for carrying out corrosion weight loss test is processed into the rectangular of required size
Body is polishing to 800~1200# step by step through sand paper, then acetone oil removing, then moves into absolute ethyl alcohol and impregnate 2~5 minutes, takes out
And cold wind dries up, and is stored in drier after package, weighs after 24~48 hours for use.
(2) etchant solution is poured into five mouthfuls of flasks 2, by Section II auxiliary electrode 3, Section II working electrode 4, Section II reference electricity
Pole 5, thermometer 6 are fixed on rubber stopper in five mouthfuls of flasks 2, make Section II auxiliary electrode and Section II reference electrode to be immersed in corrosion molten
In liquid, Section II working electrode is totally submerged in etchant solution, and then five mouthfuls of flasks 2 are fixed in digital display oil bath pan 1, by
II auxiliary electrodes 3, Section II working electrode 4, Section II reference electrode 5 are connected respectively with electrochemical test 23, carry out acid water-soluble
Electro-chemical test under pendular ring border;
Other two mouth of (3) five mouthfuls of flasks 2 connects horizontal 21 import of inner tube of condenser pipe and the horizontal inner tube of condenser pipe respectively
21 outlets, the horizontal inner tube 21 of condenser pipe is internally provided with corrosion coupon stent, by corrosion coupon 12 with being fixed on corrosion coupon branch
On frame, thermometer 10,11,13 is inserted under the input end, the port of export and condenser pipe inclined tube 14 of the horizontal inner tube 21 of condenser pipe respectively
In the thermometer socket in portion, I auxiliary electrode 17, I working electrode 18, I reference electrode 19 are fixed on condenser pipe inclined tube
Then 14 top is connect with electrochemical test 22, carry out the electro-chemical test under moisture condensation environment, then by condenser pipe level
Other two mouth of the both ends of inner tube 21 respectively with five mouthfuls of flasks 2 is connected, and fixed condenser pipe.
(4) dew-point temperature of etchant solution is calculated, digital display oil bath pan is opened and heats five mouthfuls of flasks 2, corrosive medium is made to boil,
Generate etchant gas and steam, open I section condenser pipe outer tube 7 cooling water inlet 8 and Section II section condenser pipe outer tube 20 it is cold
But water inlet 15, cooling water are entered by cooling water inlet 8 and 15, are flowed out from cooling water outlet 9 and 16, regulate the stream of cooling water
Amount makes corrosive vapor be condensed in corrosion coupon 12 and 18 surface of Section II working electrode, carries out the electricity under acidic aqueous solution at this time
The electro-chemical test experiment under corrosion weight loss experiment and moisture condensation environment under test chemical, moisture condensation environment.
The material of the corrosion sample of working electrode and the corrosion weight loss experiment of electro-chemical test can be changed as needed
Become.The ingredient and concentration of corrosive medium can be changed, to study the dew point corrosion under different condition.Experimental period can be adjusted arbitrarily
Whole, the corrosion coupon that can use 1h, 2h, 3h, 5h, 8h carries out point of XRD (X-ray diffraction), SEM (scanning electron microscope) etc.
Analysis, and be compared with Electrochemical results, carry out the research of dew point corrosion mechanism.
Claims (4)
1. a kind of distilling apparatus overhead system dew point corrosion test method, it is characterised in that include the following steps:
1) preparation of two sets of electrochemical working electrodes:It will carry out the I working electrode of electro-chemical test and Section II working electrode point
It is not processed into the cylinder of a diameter of 10~12mm, after applying envelope, solidification, polishing, polishing, oil removing and drying are spare;
The preparation of corrosion weight loss lacing film:The corrosion coupon for carrying out weightless test is processed into cuboid, then polishes, removes step by step
Oil, then move into absolute ethyl alcohol and impregnate 2~5 minutes, it takes out and dry, weighs after 24~48 hours for use;
2) etchant solution is poured into five mouthfuls of flasks, by prepared by Section II auxiliary electrode, step 1) Section II working electrode, Section II
Reference electrode and thermometer are fixed in three mouths of five mouthfuls of flasks, and Section II auxiliary electrode and Section II reference electrode is made to be immersed in corruption
It losing in solution, Section II working electrode is totally submerged in etchant solution, and then five mouthfuls of flasks are fixed in digital display oil bath pan, the
II auxiliary electrodes, Section II working electrode and Section II reference electrode are connected with electrochemical test, carry out under acidic aqueous solution environment
Electro-chemical test;
3) other two mouth of five mouthfuls of flasks connects the horizontal inner tube import of condenser pipe and the horizontal inner tube outlet of condenser pipe respectively, condensation
The horizontal internal tube of pipe is provided with corrosion coupon stent, and the corrosion coupon prepared by step 1) is placed on corrosion coupon stent
On, it is fixed, it is inserted into temperature in the input end of the horizontal inner tube of condenser pipe, the port of export and the thermometer socket of condenser pipe inclined tube lower part
I working electrode, I reference electrode prepared by I auxiliary electrode, step 1) is fixed on the top of condenser pipe inclined tube by meter,
Carry out the electro-chemical test under moisture condensation environment with electrochemical test, then by the both ends of the horizontal inner tube of condenser pipe respectively with five mouthfuls
Two mouths of flask are connected, and fixed condenser pipe;
(4) dew-point temperature of etchant solution is calculated, digital display oil bath pan is opened and heats five mouthfuls of flasks, corrosive medium is made to boil, generate
Etchant gas and steam open the cooling water inlet of I section condenser pipe outer tube and the cooling water inlet of Section II section condenser pipe outer tube,
Cooling water is entered by cooling water inlet, is flowed out from cooling water outlet, adjusts the flow of cooling water, and corrosive vapor is made to be hung in corrosion
Piece and the condensation of I working electrode surface carry out the electro-chemical test under acidic aqueous solution, the corrosion weight loss under moisture condensation environment at this time
Electro-chemical test experiment under experiment and moisture condensation environment.
2. a kind of distilling apparatus overhead system dew point corrosion test method according to claim 1, it is characterised in that:It is described
The corrosion coupon material phase of prepared I working electrode and Section II working electrode with carrying out corrosion weight loss experiment in step 1)
Together.
3. a kind of distilling apparatus overhead system dew point corrosion test method according to claim 1, it is characterised in that:It is described
It is epoxy resin that material used in envelope is applied in step 1), and oil removing material therefor is acetone.
4. a kind of distilling apparatus overhead system dew point corrosion test method according to claim 1, it is characterised in that:It is described
Polishing described in step 1) is to be polishing to 800~1200# step by step with sand paper.
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CN114428051A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Dew point corrosion assessment device with controllable condensation temperature |
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