CN105277482A - Distillation apparatus tower top system dew point corrosion test method - Google Patents
Distillation apparatus tower top system dew point corrosion test method Download PDFInfo
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- CN105277482A CN105277482A CN201410335907.3A CN201410335907A CN105277482A CN 105277482 A CN105277482 A CN 105277482A CN 201410335907 A CN201410335907 A CN 201410335907A CN 105277482 A CN105277482 A CN 105277482A
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Abstract
The present invention discloses a distillation apparatus tower top system dew point corrosion test method. The method is as follows: 1) processing a working electrode and a corrosion coupon; 2) an etching solution is poured into a five-necked flask, a second (II) three-electrode system is fixed in three mouths of the five-necked flask, the five-necked flask is fixed in a numeric display oil bath pot; 3) other two ports of the five-necked flask are respectively connected with an inlet and an outlet of a condenser horizontal inner tube, the corrosion coupon is fixed in the condenser horizontal inner tube, a first (I)three-electrode system is fixed in the upper portion of a condenser inclined tube; and 4) the five-necked flask is heated by the numeric display oil bath pot, a first-section condenser outer tube cooling water inlet and a second-section condenser outer tube cooling water outer are opened, the cooling water flow is adjusted, then acidic aqueous electrochemical tests, corrosion weight loss experiments under dew formation environment and electrochemical test experiments under dew formation environment can be performed. The electrochemical test and corrosion weight loss dew point corrosion test are can be performed by the method, tests of electrochemical impedance spectroscopy, electrochemical noise and the like under dew point environment can be realized, and data reliability can be verified by weight loss experiments.
Description
Technical field
The present invention designs a kind of distilling apparatus overhead system dew point corrosion method of testing and device, more particularly relates to a kind of method and the device that can realize the distilling apparatus overhead system dew point corrosion test of electro-chemical test and corrosion weight loss.
Background technology
Dew point corrosion is cooled to liquid by saturated vapour and material is caused to a kind of corrosion phenomenon of corrosion.The occurring in the first coagulation zone of tower top and condensing cooling system or there is the region of partial condensation of distilling apparatus tower top dew point corrosion, in tower top oil gas, most HCl enters in initial stage condensate water, the concentration forming hydrochloric acid solution can up to 1 ~ 2wt%, make the pH value of dew point position condensate water very low, formed " hcl corrosion environment " that a corrosivity is very strong.The HCl that ordinary decompression column top system occurs is from hydrolysis muriatic in crude oil.In crude oil, chloride can be divided into inorganic chlorine and organochlorine two class.Inorganic villaumite mainly contains NaCl, MgCl
2and CaCl
2, hydrolysis temperature and the degree of three kinds of inorganic salts are different.350 DEG C time, MgCl
2and CaCl
2percent hydrolysis be respectively 95% and about 10%; NaCl approximately only has 2% to decompose.
At the dew point position of overhead system, neutralizing agent NH
3not soluble in water, therefore the pH value at dew point position is not affected, do not have neutralization.Along with the reduction of system temperature, the amount of condensate water constantly increases, because HCl is constantly diluted and NH
3the increase of meltage, makes the pH value of aqueous phase raise.In Atmospheric vacuum tower top gun barrel, the pH value of condensate water can not reflect the pH value situation of whole overhead system condensate water, and this is also the reason that dew point corrosion is called the most heavy corrosion of distilling apparatus overhead system.Dew point corrosion situation is by the impact of the corrosion resistance of chlorine ion concentration, pH value, oxygen content, environment temperature and the equipment steel in condensed fluid, therefore be complicated in the dew point corrosion of the condensate cooler of atmospheric unit tower top, so high requirement is proposed to the formation of dew point corrosion and monitoring.
At present, what the domestic dew point corrosion behavior for material was reported is less.Patent CN101251467A and CN101876622A respectively with sulphuric dioxide and sulfuric anhydride for medium, describe a kind of proving installation and method of testing thereof of evaluating material sulfuric-resisting dew point corrosion performance quality, by being that weight-loss method is evaluated, corrosion environment and the actual dew point corrosion environment of simulation are comparatively close, shortcoming can not carry out the electro-chemical test such as electrochemical impedance spectroscopy, electrochemistry noise in the present context, means are single, are unfavorable for dew point corrosion study mechanism.Patent CN101929945A to describe in a kind of yellow phosphoric tail gas phosphorus to the low-temperature dew point corrosion experimental technique of boiler material and device, material is invaded bubble certain hour by this invention in the phosphoric acid solution of different temperatures variable concentrations, the dew point corrosion performance of evaluating material is carried out by the weight change of material before and after soaking, corrosion environment departs from actual dew point corrosion environment, have ignored the condensation of acid, come off and the actual dew point corrosion environment such as coagulative diffusion, the data obtained reliability is still to be tested.Patent CN102692438A invents a kind of dew point corrosion experiment device that can realize electro-chemical test, but can not carry out corrosion weight loss experiment simultaneously, and the reliability of data is not verified by corrosion weight loss.
Summary of the invention
The object of this invention is to provide a kind of distilling apparatus overhead system dew point corrosion method of testing, the method can carry out the dew point corrosion test that electro-chemical test can carry out again corrosion weight loss, achieve the tests such as the electrochemical impedance spectroscopy of material under dew point environment, electrochemistry noise, the reliability of data can be verified by weightless test again.
The invention provides a kind of distilling apparatus overhead system dew point corrosion method of testing, it is characterized in that comprising the steps:
1) two cover electrochemical working electrodes preparation: the I working electrode and II working electrode that carry out electro-chemical test are processed into the right cylinder that diameter is 10 ~ 12mm respectively, be coated with envelope, solidify after, polishing, polishing, oil removing and drying, for subsequent use;
The preparation of corrosion weight loss lacing film: the corrosion coupon carrying out weightless test is processed into rectangular parallelepiped, then polishes step by step, oil removing, then move in absolute ethyl alcohol and soak 2 ~ 5 minutes, takes out and dry, weighs stand-by after 24 ~ 48 hours;
2) etchant solution is poured in five mouthfuls of flasks, by II auxiliary electrode, step 1) prepared by II working electrode, II contrast electrode and thermometer be fixed in three mouths of five mouthfuls of flasks, II auxiliary electrode and II contrast electrode is made to be immersed in etchant solution, II working electrode is submerged in etchant solution completely, then five mouthfuls of flasks are fixed in digital display oil bath pan, II auxiliary electrode, II working electrode are connected with electrochemical test with II contrast electrode, carry out the electro-chemical test under acidic aqueous solution environment;
3) two other mouth of five mouthfuls of flasks connects pipe import and the horizontal inner tube outlet of condenser pipe in condenser pipe level respectively, the horizontal internal tube of condenser pipe is provided with corrosion coupon support, by step 1) prepared by corrosion coupon be placed on corrosion coupon support, fixing, the entrance point of pipe in condenser pipe level, all thermometer is inserted in the thermometer socket of endpiece and condenser pipe inclined tube bottom, by I auxiliary electrode, step 1) prepared by I working electrode, I contrast electrode is fixed on the top of condenser pipe inclined tube, the electro-chemical test under condensation environment is carried out with electrochemical test, then the two ends of pipe in condenser pipe level are connected with two mouths of five mouthfuls of flasks respectively, and fixing condenser pipe,
(4) dewpoint temperature of etchant solution is calculated, open digital display oil bath pan and heat five mouthfuls of flasks, corrosive medium is seethed with excitement, produce etchant gas and steam, open the cooling water inlet of I section condenser pipe outer tube and the cooling water inlet of II section condenser pipe outer tube, chilled water is by cooling water inlet and enter, from coolant outlet and outflow, regulate the flow of chilled water, make corrosive vapor in corrosion coupon and the condensation of II working electrode surface, now carry out the electro-chemical test under acidic aqueous solution, corrosion weight loss experiment under condensation environment and the electro-chemical test experiment under condensation environment.
The further technical characteristic of the present invention is: described step 1) in prepared I working electrode identical with the corrosion coupon material of carrying out corrosion weight loss experiment with II working electrode.
The further technical characteristic of the present invention is: described step 1) in be coated with that to seal the material that uses be epoxy resin, oil removing material therefor is acetone.
The further technical characteristic of the present invention is: described step 1) described in polishing for polish step by step to 800 ~ 1200# with sand paper.
Present invention employs two cover electrochemical test system, test the electrochemical impedance spectroscopy under acidic aqueous solution environment and condensation environment and electrochemistry noise respectively, thus confirm the condensation environment of acidic aqueous solution environment and dew point corrosion with experiment under, the dew point corrosion mechanism of material is different, has had further understanding to dew point corrosion mechanism.
First set electrochemical test system in the present invention is used for testing electrochemical impedance spectroscopy under acidic aqueous solution environment and electrochemistry noise, comprises digital display oil bath pan, five mouthfuls of flasks, electrochemical test, thermometer and II three-electrode systems.II three-electrode system i.e. II contrast electrode, II auxiliary electrode and II working electrode, wherein II contrast electrode can be Ag/AgCl electrode, and II auxiliary electrode can be platinum electrode, and II working electrode is institute's test sample.
In the present invention second cover electrochemical test system be used for test condensation environment under electro-chemical test, comprise condenser pipe inclined tube, II section condenser pipe outer tube, thermometer, I three-electrode system and electrochemical test, I three-electrode system i.e. I contrast electrode, I auxiliary electrode and I working electrode, wherein I contrast electrode can be Ag/AgCl electrode, I auxiliary electrode can be platinum electrode, and I working electrode is institute's test sample.
Weightless test system in the present invention comprises pipe, I section condenser pipe outer tube, thermometer and corrosion coupon in condenser pipe level.
Experimental technique of the present invention is:
Put in digital display oil bath pan 1 by the five mouthfuls of flasks 2 filling etchant solution, digital display oil bath pan heating corrosive medium, makes it boiling, produces acid medium and steam.Be fixed in five mouthfuls of flasks by II auxiliary electrode 3, II working electrode 4, II contrast electrode 5, thermometer 6 rubber plug, make it to be immersed in solution, II working electrode 4 will be submerged in corrosive liquid completely.In condenser pipe level, the two ends of pipe 2I are connected with two mouths of five mouthfuls of flasks 2 respectively, realize the circulation of solution, ensure the consistance of corrosive medium in whole experimentation.By one group of (6) parallel corrosion coupon 12, fix with test piece frame, to be placed in condenser pipe level in pipe 21.Thermometer 10,11,13 is inserted respectively in the thermometer socket of the entrance point of pipe 21 in condenser pipe level, endpiece and condensation inclined tube 14 bottom, to monitor the temperature of whole experimentation, determine the experiment carried out under the condition of dew point.The chilled water of I section condenser pipe outer tube 7 and II section condenser pipe outer tube 20 enters from mouth 8,15 respectively, flow out from 9,16, two-way chilled water can ensure that etchant gas total condensation is got off, make it to be back in five mouthfuls of flasks, and the flow of chilled water will be regulated according to thermometer, carry out under guaranteeing to test tangible condensation condition.Carry out another set of electrochemical test system on the top, another port of condensation inclined tube 14, II auxiliary electrode 17, II working electrode 18, II contrast electrode 19 are fixed on the port of condensation inclined tube 14, the electro-chemical test under the environment that carries out condensing.
This experimental technique is not only confined to the research of distilling the dew point corrosion of tower top hydrochloric acid, can change corrosive medium as required, the dew point corrosion of corrosive medium such as research sulfuric acid, phosphoric acid etc.
The invention has the advantages that: 1. the corrosion environment of the present invention's simulation is comparatively close with actual dew point corrosion environment, and can carry out electro-chemical test.2. the present invention is provided with two cover electrochemical test system, test the electrochemical impedance spectroscopy under acidic aqueous solution environment and condensation environment and electrochemistry noise respectively, under can confirming the condensation environment of acidic aqueous solution environment and dew point corrosion with experiment, the corrosion mechanism of material is likely different.3. the present invention is provided with corrosion weight loss experiment, and the result of electro-chemical test can be verified by weightless test.The present invention carries out under close dew temperature, normal pressure, simple to operate, and security is higher, and realizes closed circulation, does not produce pollution.
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, but does not limit the scope of the invention.
Accompanying drawing explanation
Fig. 1 is a kind of distilling apparatus overhead system of the present invention dew point corrosion method of testing schematic flow sheet.
Reference numeral shown in figure is:
1-digital display oil bath pan; 2-five mouthfuls of flasks; 3-II auxiliary electrode; 4-II working electrode; 5-II contrast electrode; 6,10,11,13-thermometer; 7-I section condenser pipe outer tube; 14-condenser pipe inclined tube; 8,15-cooling water inlet; 9,16-coolant outlet; 12-corrosion coupon, 17-I auxiliary electrode; 18-I working electrode; 19-I contrast electrode; 20-II section condenser pipe outer tube; Pipe in 21-condenser pipe level; 22,23-electrochemical test.
Embodiment
As shown in Figure 1, a kind of distilling apparatus overhead system dew point corrosion method of testing.The steps include:
(1) preparation of the working electrode of electro-chemical test: will the working electrode of electro-chemical test be carried out, i.e. I working electrode and II working electrode, is processed into the right cylinder that diameter is 10 ~ 12mm, welds with welding rod, then envelope is coated with epoxy resin, after solidifying, abrasive paper for metallograph is polished step by step to 800 ~ 1200#, then carries out polishing, acetone oil removing, with the wiping of anhydrous alcohol cotton balls, hair dryer dries up, and puts into drying box for subsequent use;
The preparation of corrosion weight loss lacing film: the rectangular parallelepiped corrosion coupon carrying out corrosion weight loss test being processed into required size, polish step by step to 800 ~ 1200# through sand paper, then acetone oil removing, move into again in absolute ethyl alcohol and soak 2 ~ 5 minutes, take out also cold wind to dry up, be stored in after parcel in exsiccator, weigh after 24 ~ 48 hours stand-by.
(2) etchant solution is poured in five mouthfuls of flasks 2, II auxiliary electrode 3, II working electrode 4, II contrast electrode 5, thermometer 6 rubber plug are fixed in five mouthfuls of flasks 2, II auxiliary electrode and II contrast electrode is made to be immersed in etchant solution, II working electrode is submerged in etchant solution completely, then five mouthfuls of flasks 2 are fixed in digital display oil bath pan 1, II auxiliary electrode 3, II working electrode 4, II contrast electrode 5 are connected with electrochemical test 23 respectively, carry out the electro-chemical test under acidic aqueous solution environment;
Two other mouths of (3) five mouthfuls of flasks 2 to connect in condenser pipe level pipe 21 in pipe 21 import and condenser pipe level respectively and exports, in condenser pipe level, pipe 21 inside is provided with corrosion coupon support, by corrosion coupon 12 with being fixed on corrosion coupon support, by thermometer 10, 11, 13 entrance points inserting pipe 21 in condenser pipe level respectively, in the thermometer socket of endpiece and condenser pipe inclined tube 14 bottom, by I auxiliary electrode 17, I working electrode 18, I contrast electrode 19 is fixed on the top of condenser pipe inclined tube 14, then be connected with electrochemical test 22, carry out the electro-chemical test under condensation environment, then the two ends of pipe 21 in condenser pipe level are connected with two other mouth of five mouthfuls of flasks 2 respectively, and fixing condenser pipe.
(4) dewpoint temperature of etchant solution is calculated, open digital display oil bath pan and heat five mouthfuls of flasks 2, corrosive medium is seethed with excitement, produce etchant gas and steam, open the cooling water inlet 8 of I section condenser pipe outer tube 7 and the cooling water inlet 15 of II section condenser pipe outer tube 20, chilled water is entered by cooling water inlet 8 and 15, flow out from coolant outlet 9 and 16, regulate the flow of chilled water, make corrosive vapor in corrosion coupon 12 and II working electrode 18 surface condensation, now carry out the electro-chemical test under acidic aqueous solution, corrosion weight loss experiment under condensation environment and the electro-chemical test experiment under condensation environment.
The material of the corrosion sample of the working electrode of electro-chemical test and corrosion weight loss experiment can change as required.Composition and the concentration of corrosive medium can be changed, to study the dew point corrosion under different condition.Experimental period can arbitrarily adjust, the corrosion coupon of desirable 1h, 2h, 3h, 5h, 8h carries out the analysis of XRD (X-ray diffraction), SEM (scanning electron microscope) etc., and compare with Electrochemical results, carry out the research of dew point corrosion mechanism.
Claims (4)
1. a distilling apparatus overhead system dew point corrosion method of testing, is characterized in that comprising the steps:
1) two cover electrochemical working electrodes preparation: the I working electrode and II working electrode that carry out electro-chemical test are processed into the right cylinder that diameter is 10 ~ 12mm respectively, be coated with envelope, solidify after, polishing, polishing, oil removing and drying, for subsequent use;
The preparation of corrosion weight loss lacing film: the corrosion coupon carrying out weightless test is processed into rectangular parallelepiped, then polishes step by step, oil removing, then move in absolute ethyl alcohol and soak 2 ~ 5 minutes, takes out and dry, weighs stand-by after 24 ~ 48 hours;
2) etchant solution is poured in five mouthfuls of flasks, by II auxiliary electrode, step 1) prepared by II working electrode, II contrast electrode and thermometer be fixed in three mouths of five mouthfuls of flasks, II auxiliary electrode and II contrast electrode is made to be immersed in etchant solution, II working electrode is submerged in etchant solution completely, then five mouthfuls of flasks are fixed in digital display oil bath pan, II auxiliary electrode, II working electrode are connected with electrochemical test with II contrast electrode, carry out the electro-chemical test under acidic aqueous solution environment;
3) two other mouth of five mouthfuls of flasks connects pipe import and the horizontal inner tube outlet of condenser pipe in condenser pipe level respectively, the horizontal internal tube of condenser pipe is provided with corrosion coupon support, by step 1) prepared by corrosion coupon be placed on corrosion coupon support, fixing, the entrance point of pipe in condenser pipe level, all thermometer is inserted in the thermometer socket of endpiece and condenser pipe inclined tube bottom, by I auxiliary electrode, step 1) prepared by I working electrode, I contrast electrode is fixed on the top of condenser pipe inclined tube, the electro-chemical test under condensation environment is carried out with electrochemical test, then the two ends of pipe in condenser pipe level are connected with two mouths of five mouthfuls of flasks respectively, and fixing condenser pipe,
4) dewpoint temperature of etchant solution is calculated, open digital display oil bath pan and heat five mouthfuls of flasks, corrosive medium is seethed with excitement, produce etchant gas and steam, open the cooling water inlet of I section condenser pipe outer tube and the cooling water inlet of II section condenser pipe outer tube, chilled water is by cooling water inlet and enter, from coolant outlet and outflow, regulate the flow of chilled water, make corrosive vapor in corrosion coupon and the condensation of II working electrode surface, now carry out the electro-chemical test under acidic aqueous solution, corrosion weight loss experiment under condensation environment and the electro-chemical test experiment under condensation environment.
2. a kind of distilling apparatus overhead system dew point corrosion method of testing according to claim 1, is characterized in that: described step 1) in prepared I working electrode identical with the corrosion coupon material of carrying out corrosion weight loss experiment with II working electrode.
3. a kind of distilling apparatus overhead system dew point corrosion method of testing according to claim 1, is characterized in that: described step 1) in be coated with that to seal the material that uses be epoxy resin, oil removing material therefor is acetone.
4. a kind of distilling apparatus overhead system dew point corrosion method of testing according to claim 1, is characterized in that: described step 1) described in polishing for polish step by step to 800 ~ 1200# with sand paper.
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| CN106950145A (en) * | 2017-03-07 | 2017-07-14 | 河南师范大学 | Suitable for the dynamic experiment method and apparatus of recirculating cooling water system pipeline scale |
| CN108037067A (en) * | 2018-01-08 | 2018-05-15 | 中国科学院金属研究所 | Simulation of desulfurization flue gas apparatus dew point corrodes and realizes the experimental provision of electro-chemical test |
| CN108344784A (en) * | 2018-02-07 | 2018-07-31 | 东南大学 | A kind of vacuum condensing system with corrosion of piping on-Line Monitor Device |
| CN109988595A (en) * | 2018-01-02 | 2019-07-09 | 中国石油天然气股份有限公司 | The screening technique of the very useful compound neutralizer of fractionating column in a kind of crude distillation |
| CN110420607A (en) * | 2019-08-19 | 2019-11-08 | 遵义师范学院 | Material corrosion behavioral study device and its reaction kettle in hydrothermal system |
| CN111595719A (en) * | 2020-05-27 | 2020-08-28 | 中国石油化工股份有限公司 | Evaluation device and corrosion inhibition performance evaluation method for vapor phase corrosion inhibitor on top of distillation tower |
| 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 |
| CN113412421A (en) * | 2018-07-31 | 2021-09-17 | 沙特阿拉伯石油公司 | Method for generating and testing aqueous gas streams |
| CN113848174A (en) * | 2021-10-13 | 2021-12-28 | 中国核动力研究设计院 | Electrochemical corrosion test device in boiling and strong corrosive solution environment and application thereof |
| 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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| CN106556549A (en) * | 2016-10-28 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of method and apparatus of oil plant air-distillation column overhead scaling rate test |
| CN106556549B (en) * | 2016-10-28 | 2019-07-19 | 中国石油化工股份有限公司 | A kind of method and apparatus of oil plant air-distillation column overhead scaling rate test |
| CN106950145A (en) * | 2017-03-07 | 2017-07-14 | 河南师范大学 | Suitable for the dynamic experiment method and apparatus of recirculating cooling water system pipeline scale |
| CN109988595B (en) * | 2018-01-02 | 2021-04-30 | 中国石油天然气股份有限公司 | Screening method of composite neutralizer for fractionating tower top in crude oil distillation |
| CN109988595A (en) * | 2018-01-02 | 2019-07-09 | 中国石油天然气股份有限公司 | The screening technique of the very useful compound neutralizer of fractionating column in a kind of crude distillation |
| CN108037067A (en) * | 2018-01-08 | 2018-05-15 | 中国科学院金属研究所 | Simulation of desulfurization flue gas apparatus dew point corrodes and realizes the experimental provision of electro-chemical test |
| CN108344784A (en) * | 2018-02-07 | 2018-07-31 | 东南大学 | A kind of vacuum condensing system with corrosion of piping on-Line Monitor Device |
| CN113412421A (en) * | 2018-07-31 | 2021-09-17 | 沙特阿拉伯石油公司 | Method for generating and testing aqueous gas streams |
| CN110420607A (en) * | 2019-08-19 | 2019-11-08 | 遵义师范学院 | Material corrosion behavioral study device and its reaction kettle in hydrothermal system |
| CN111595719A (en) * | 2020-05-27 | 2020-08-28 | 中国石油化工股份有限公司 | Evaluation device and corrosion inhibition performance evaluation method for vapor phase corrosion inhibitor on top of distillation tower |
| 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 |
| 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 |
| CN113848174A (en) * | 2021-10-13 | 2021-12-28 | 中国核动力研究设计院 | Electrochemical corrosion test device in boiling and strong corrosive solution environment and application thereof |
| CN113848174B (en) * | 2021-10-13 | 2023-11-10 | 中国核动力研究设计院 | Electrochemical corrosion test device under boiling and strong corrosive solution environment and application thereof |
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