CN108051365A - High temperature and pressure hydrogen diffusion test set - Google Patents
High temperature and pressure hydrogen diffusion test set Download PDFInfo
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- CN108051365A CN108051365A CN201810018696.9A CN201810018696A CN108051365A CN 108051365 A CN108051365 A CN 108051365A CN 201810018696 A CN201810018696 A CN 201810018696A CN 108051365 A CN108051365 A CN 108051365A
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- Prior art keywords
- high temperature
- sample holder
- pressure
- test set
- seal
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 35
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 34
- 238000009792 diffusion process Methods 0.000 title claims abstract description 18
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title description 3
- 238000007789 sealing Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 15
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 8
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000009434 installation Methods 0.000 abstract description 3
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical compound [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 230000008595 infiltration Effects 0.000 description 4
- 238000001764 infiltration Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
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- Life Sciences & Earth Sciences (AREA)
- Biodiversity & Conservation Biology (AREA)
- Ecology (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
High temperature and pressure hydrogen diffusion test set including a high temperature and high pressure kettle, radially sets a sealing shroud on the side wall of high temperature and high pressure kettle；One end of sealing shroud is located in the reaction chamber of high temperature and high pressure kettle, and the other end protrudes out the lateral wall of high temperature and high pressure kettle；Sample holder is embedded in sealing shroud, is tightly connected between sample holder and the lateral wall of high temperature and high pressure kettle；The inner end of sample holder is connected with reaction chamber；The inner cavity of sample holder is connected with anode evolving hydrogen reaction slot；The side of sample holder is connected using hard sealing means with high temperature and high pressure kettle；The front end of sample holder sets seal and polytetrafluoro pressure ring, sample to be placed between polytetrafluoro pressure ring and seal；The conducting wire of sample is connected through seal, leads to outside sample holder and is connected with electrochemical workstation；The side wall of anode evolving hydrogen reaction slot is equipped with reference electrode, auxiliary electrode, and reference electrode, auxiliary electrode are connected with electrochemical workstation；Have the characteristics that simple in structure, easy for installation, detection is not omitted comprehensively.
Description
Technical field
The invention belongs to oil country tubular good Corrosion monitoring technical fields, and in particular to high temperature and pressure hydrogen diffusion test set.
Background technology
At present, room temperature hydrogen permeability apparatus is sealed using resistance to hydrogen sulfide O-ring seal, and is fixed using dedicated metal clip
Sample；Metal material is detected in high temperature and pressure hydrogen sulfide（H2S）Hydrogen infiltration capacity in sour environment.However for Hi-grade steel oil jacket
The detection of the hydrogen infiltration capacity of tube steel is but without preferable solution.
The content of the invention
To overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide high temperature and pressure hydrogen diffusion test set, tools
There is the characteristics of simple in structure, easy for installation, detection is not omitted comprehensively.
To achieve the above object, the technical solution adopted by the present invention is：High temperature and pressure hydrogen diffusion test set is high including one
Warm autoclave radially sets a sealing shroud on the side wall of high temperature and high pressure kettle；One end of sealing shroud is located at high temperature and high pressure kettle
Reaction chamber in, the other end protrudes out the lateral wall of high temperature and high pressure kettle；Sample holder is embedded in sealing shroud, and sample holder is high with high temperature
It is tightly connected between the lateral wall of pressure kettle；The inner end of sample holder is connected with reaction chamber；The inner cavity of sample holder and anode liberation of hydrogen
Reactive tank is connected；The side of sample holder is connected using hard sealing means with high temperature and high pressure kettle；The front end of sample holder sets insulation
Device and polytetrafluoro pressure ring, sample are placed between polytetrafluoro pressure ring and seal；The conducting wire for connecting sample passes through seal,
It leads to outside sample holder and is connected with electrochemical workstation；The side wall of anode evolving hydrogen reaction slot is equipped with reference electrode 9, auxiliary electricity
Pole, reference electrode, auxiliary electrode are connected with electrochemical workstation.
The high temperature and high pressure kettle uses TFCZ-35/250 type high temperature and pressure cathode reaction kettles.
The sealing shroud and the reaction chamber of high temperature and high pressure kettle, the outer wall of high temperature and high pressure kettle are tightly connected.
The seal is made of polytetrafluoroethylene (PTFE).
The conductive line surfaces insulation.
The sample, reference electrode, auxiliary electrode form three-electrode system.
The sealing ring is sealed using resistance to hydrogen sulfide O-ring seal.
The beneficial effects of the invention are as follows：
Compared with prior art, the present invention is according to Devnathan-Stachurski double-electrolyzer model diffusion principles, using electricity
Chemistry oozes the hydrogen infiltration capacity of hydrogen method acquisition hydrogenation electric current detection Hi-grade steel oil annular tube steel；It is close using resistance to hydrogen sulfide O-ring seal
Envelope, and sample is fixed using dedicated metal clip；In order to detect metal material in high temperature and pressure hydrogen sulfide（H2S）In sour environment
Hydrogen infiltration capacity；The conducting wire of connection sample, which is led to by seal outside sample holder, to be connected on electrochemical workstation, conducting wire
Surface insulation.Reference electrode, auxiliary electrode are placed in anode evolving hydrogen reaction slot, and together with sample with electrochemical workstation phase
Even, three-electrode system is formed.The hydrogen that solving the prior art can only detect under room temperature is spread, and cannot detect hydrogen under high temperature and pressure
Spread the technical barrier of test.Have the characteristics that simple in structure, easy for installation, detection is accurate.
Description of the drawings
Fig. 1 is the overall structure diagram of the present invention.
Fig. 2 is the section components structure diagram of the present invention.
Specific embodiment
The structural principle and operation principle of the present invention are described in further detail with reference to the accompanying drawings and examples.
Referring to Fig. 1,2, high temperature and pressure hydrogen diffusion test set, including a high temperature and high pressure kettle 1, on the side wall of high temperature and high pressure kettle
One sealing shroud 2 is radially set；One end of sealing shroud 2 is located in the reaction chamber 3 of high temperature and high pressure kettle, and the other end protrudes out height
The lateral wall of warm autoclave；Sample holder 4 is embedded in sealing shroud, the company of sealing between sample holder and the lateral wall of high temperature and high pressure kettle
It connects；The inner end of sample holder is connected with reaction chamber；The inner cavity of sample holder 4 is connected with anode evolving hydrogen reaction slot 5；Sample holder exists
Side is connected using hard sealing means with high temperature and high pressure kettle；The front end of sample holder sets seal 6 and polytetrafluoro pressure ring 7, examination
Sample is placed between polytetrafluoro pressure ring 7 and seal 6；The conducting wire 8 of sample 11 is connected through seal, is led to outside sample holder
It is connected with electrochemical workstation 11；The side wall of anode evolving hydrogen reaction slot 5 is equipped with reference electrode 9, auxiliary electrode 10, reference electrode
9th, auxiliary electrode 10 is connected with electrochemical workstation 12.
The high temperature and high pressure kettle uses TFCZ-35/250 type high temperature and pressure cathode reaction kettles.
The sealing shroud 2 is tightly connected with the reaction chamber of high temperature and high pressure kettle, the outer wall of high temperature and high pressure kettle.
The seal 6 is made of composite material polytetrafluoroethylene (PTFE).
8 surface insulation of conducting wire.
The sample, reference electrode 9, auxiliary electrode 10 form three-electrode system.
The sealing ring is sealed using resistance to hydrogen sulfide O-ring seal
The present invention operation principle be：
Measuring device is made of two mutually different electrolytic cells, and high temperature and high pressure kettle end is hydrogen-filling chamber（Cathode chamber）, electrolysis fills
The left side of sample is the cathode current i applied during hydrogenc, react, a hydrogen atom part for generation
It synthesizes hydrogen molecule to release, another part is diffused into inside sample, and sample right end is the anode of another electrolytic cell, when plus anode
After constant potential, expand the hydrogen atom come from the diffusion of sample left side and aoxidized on the right side of sample, i.e.,,
So as to generate anode current.
It is reacted if there is no surface（By plating palladium or nickel plating on carbon steel surface and adding
Upper sufficiently large anode potential can inhibit the progress of surface reaction）, then generated after a period of time on the left of sample
Atomic hydrogen on the right side of the arrival after will all be aoxidized, i.e., the concentration C of upper atomic hydrogen on the right side of sampleA=0, the at this moment oxidation of atomic hydrogen
Electric current Ia reaches maximum as steady-state current density, is represented with Imax.Therefore when reaching stable state, obtained according to Fick First Laws
In formula：F is Faraday constant；D is diffusion coefficient；Δ x=L, for the thickness of sample, CA=C1=0, because H is former on the right side of sample
Son is all oxidized to H+;C0=CCTo be flushed with hydrogen end concentration, when be flushed with hydrogen electric current Ic it is constant when, it is also constant, therefore above formula can be write
Into：
By measuring current density Imax, then the concentration of the atomic hydrogen in tapping can be calculated.
Claims (8)
1. high temperature and pressure hydrogen diffusion test set, including a high temperature and high pressure kettle（1）, which is characterized in that the side wall of high temperature and high pressure kettle
On a sealing shroud is radially set（2）；Sealing shroud（2）One end be located at the reaction chamber of high temperature and high pressure kettle（3）It is interior, the other end
Protrude out the lateral wall of high temperature and high pressure kettle；Sample holder（4）Be embedded in sealing shroud, the lateral wall of sample holder and high temperature and high pressure kettle it
Between be tightly connected；The inner end of sample holder is connected with reaction chamber；Sample holder（4）Inner cavity and anode evolving hydrogen reaction slot（5）Phase
Connection；The side of sample holder is connected using hard sealing means with high temperature and high pressure kettle；The front end of sample holder sets seal（6）With
Polytetrafluoro pressure ring（7）, sample is placed in polytetrafluoro pressure ring（7）And seal（6）Between；Connect sample（11）Conducting wire（8）It wears
Seal is crossed, leads to that sample holder is outer and electrochemical workstation（11）It is connected；Anode evolving hydrogen reaction slot（5）Side wall be equipped with
Reference electrode（9）, auxiliary electrode（10）, reference electrode（9）, auxiliary electrode（10）With electrochemical workstation（12）It is connected.
2. high temperature and pressure hydrogen diffusion test set according to claim 1, which is characterized in that the high temperature and high pressure kettle is adopted
With TFCZ-35/250 type high temperature and pressure cathode reaction kettles.
3. high temperature and pressure hydrogen diffusion test set according to claim 1, which is characterized in that the sealing shroud 2 and height
The reaction chamber of warm autoclave, the outer wall of high temperature and high pressure kettle are tightly connected.
4. high temperature and pressure hydrogen diffusion test set according to claim 1, which is characterized in that the seal（7）
It is made of polytetrafluoroethylene (PTFE).
5. high temperature and pressure hydrogen diffusion test set according to claim 1, which is characterized in that the conducting wire（8）Surface
Insulation.
6. high temperature and pressure hydrogen diffusion test set according to claim 1, which is characterized in that the sample, reference electricity
Pole（9）, auxiliary electrode（10）Form three-electrode system.
7. high temperature and pressure hydrogen diffusion test set according to claim 1, which is characterized in that the seal（6）
It is sealed using resistance to hydrogen sulfide O-ring seal.
8. high temperature and pressure hydrogen diffusion test set according to claim 7, which is characterized in that the sealing ring is using resistance to
Hydrogen sulfide O-ring seal seals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810018696.9A CN108051365A (en) | 2018-01-09 | 2018-01-09 | High temperature and pressure hydrogen diffusion test set |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810018696.9A CN108051365A (en) | 2018-01-09 | 2018-01-09 | High temperature and pressure hydrogen diffusion test set |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108051365A true CN108051365A (en) | 2018-05-18 |
Family
ID=62126021
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810018696.9A Withdrawn CN108051365A (en) | 2018-01-09 | 2018-01-09 | High temperature and pressure hydrogen diffusion test set |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108051365A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115814702A (en) * | 2022-10-11 | 2023-03-21 | 中国石油大学(华东) | Propeller type hydrogen permeation single-window autoclave |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202693457U (en) * | 2012-08-14 | 2013-01-23 | 中国石油大学(北京) | Hydrogen penetration detecting device in high-temperature high-pressure hydrothion environment |
| CN104515732A (en) * | 2014-12-19 | 2015-04-15 | 北京科技大学 | Hydrogen permeability testing device for metal material under high liquid pressure |
| CN104880400A (en) * | 2014-12-02 | 2015-09-02 | 浙江工业大学 | High pressure hydrogen penetration test device and method |
| CN104897744A (en) * | 2015-04-23 | 2015-09-09 | 中国石油大学(华东) | Metal hydrogen permeation behavior research device and method |
| CN105842149A (en) * | 2016-03-17 | 2016-08-10 | 西南石油大学 | Detection apparatus and method for hydrogen permeation in high-temperature high-pressure hydrogen sulfide environment and under stress conditions |
| CN207908328U (en) * | 2018-01-09 | 2018-09-25 | 西安摩尔石油工程实验室股份有限公司 | High temperature and pressure hydrogen diffusion test set |
-
2018
- 2018-01-09 CN CN201810018696.9A patent/CN108051365A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202693457U (en) * | 2012-08-14 | 2013-01-23 | 中国石油大学(北京) | Hydrogen penetration detecting device in high-temperature high-pressure hydrothion environment |
| CN104880400A (en) * | 2014-12-02 | 2015-09-02 | 浙江工业大学 | High pressure hydrogen penetration test device and method |
| CN104515732A (en) * | 2014-12-19 | 2015-04-15 | 北京科技大学 | Hydrogen permeability testing device for metal material under high liquid pressure |
| CN104897744A (en) * | 2015-04-23 | 2015-09-09 | 中国石油大学(华东) | Metal hydrogen permeation behavior research device and method |
| CN105842149A (en) * | 2016-03-17 | 2016-08-10 | 西南石油大学 | Detection apparatus and method for hydrogen permeation in high-temperature high-pressure hydrogen sulfide environment and under stress conditions |
| CN207908328U (en) * | 2018-01-09 | 2018-09-25 | 西安摩尔石油工程实验室股份有限公司 | High temperature and pressure hydrogen diffusion test set |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115814702A (en) * | 2022-10-11 | 2023-03-21 | 中国石油大学(华东) | Propeller type hydrogen permeation single-window autoclave |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180518 |
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| WW01 | Invention patent application withdrawn after publication |