CN106969965A - A kind of method that electrolysis extracts carbonitride - Google Patents
A kind of method that electrolysis extracts carbonitride Download PDFInfo
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- CN106969965A CN106969965A CN201710137493.7A CN201710137493A CN106969965A CN 106969965 A CN106969965 A CN 106969965A CN 201710137493 A CN201710137493 A CN 201710137493A CN 106969965 A CN106969965 A CN 106969965A
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- carbonitride
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- inert gas
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 21
- 239000000284 extract Substances 0.000 title claims abstract description 11
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 28
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003792 electrolyte Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000005486 organic electrolyte Substances 0.000 claims abstract description 6
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 5
- 229920000515 polycarbonate Polymers 0.000 claims description 5
- 239000004417 polycarbonate Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 238000005660 chlorination reaction Methods 0.000 claims description 4
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 4
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 abstract description 3
- 230000003628 erosive effect Effects 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000008139 complexing agent Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/06—Etching of iron or steel
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N2001/4038—Concentrating samples electric methods, e.g. electromigration, electrophoresis, ionisation
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses a kind of method that electrolysis extracts carbonitride.It comprises the following steps：A, organic electrolyte is added in a cell；B, specimen surface is polished and is put into electrolytic cell after cleaning；C, inert gas is passed through, using sample as anode, platinum electrode is negative electrode；D, above-mentioned electrolyte is filtered with absolute ethyl alcohol after be put into vacuum separation filter and separate precipitate, obtain carbonitride NbC, NbN and M23C6.After adopting with the aforedescribed process, using tetramethyl ammonium chloride as surfactant, the activity on energy holding electrode surface is uniformly electrolysed, acetylacetone,2,4-pentanedione is used as complexing agent, it is therefore prevented that the Hydrolysis Reactions of Metal-ions generation complex compound of electrolysis；The addition of particularly lithium chloride makes it substantially increase catalytic reaction effect as catalyst and effectively prevent the erosion being subject in electrolytic process, in addition, various composition formula rate is appropriate so that reaction effect is good so that final product is extracted accurately and recovery rate is very high.
Description
Technical field
The present invention relates to a kind of extractive technique of metal object, specifically a kind of electrolysis extracts the side of carbonitride
Method.
Background technology
The species of carbonitride, quantity, size and distribution are to influence the key factor of ferrous materials performance in steel, carbon nitridation
The change of thing also directly influences the performance of ferrous materials；Research carbonitride is generally carried out using probe device in the prior art
Species, existing this method, due to its detection method limitation cause can only observe local region, later with electricity
The development of solution extractive technique, although carbonitride can be extracted from sample and be analyzed, but be due to its operation
Method is simultaneously unreasonable, is easily suffered erosion in electrolytic process, it is difficult to accomplish accurate extraction, reduces recovery rate.
The content of the invention
The technical problem to be solved in the present invention is can accurately to extract and electrolysis that recovery rate is high extracts carbonitride
Method.
In order to solve the above-mentioned technical problem, the method that electrolysis of the invention extracts carbonitride, comprises the following steps：
A, organic electrolyte is added in a cell；The proportioning of electrolyte is in percentage by weight：Tetramethyl ammonium chloride 2.5
~3%, acetylacetone,2,4-pentanedione 10~13%, lithium chloride 3~5%, surplus is 95~98% methanol；
B, specimen surface is polished and is put into electrolytic cell after cleaning；
C, inert gas is passed through, using sample as anode, platinum electrode is negative electrode, control electric current 15~18mA/cm2 of density, constant current
It is electrolysed 15~18h；Electrolysis temperature is 1~3 DEG C；
D, above-mentioned electrolyte is filtered with absolute ethyl alcohol after be put into vacuum separation filter and separate precipitate, obtain carbon
Nitride NbC, NbN and M23C6.
The inert gas is argon gas.
The vacuum separation filter is using polycarbonate membrane as filtration supports.
After adopting with the aforedescribed process, using tetramethyl ammonium chloride as surfactant, the activity on energy holding electrode surface is obtained
To uniform electrolysis, acetylacetone,2,4-pentanedione is used as complexing agent, it is therefore prevented that the Hydrolysis Reactions of Metal-ions generation complex compound of electrolysis；Particularly lithium chloride
Addition it is substantially increased catalytic reaction effect as catalyst and effectively prevent the erosion being subject in electrolytic process,
In addition, various composition formula rate is appropriate so that reaction effect is good so that final product extracts accurate and recovery rate very
Height, reaches more than 98%.
Embodiment
With reference to embodiment, the method to the electrolysis extraction carbonitride of the present invention is made further specifically
It is bright.
Embodiment one：
The method that the electrolysis of the present invention extracts carbonitride, comprises the following steps：
A, organic electrolyte is added in a cell；The proportioning of the electrolyte is in percentage by weight：Tetramethyl chlorination
Ammonium 2.5%, acetylacetone,2,4-pentanedione 10%, lithium chloride 3%, surplus is 95% methanol；
B, specimen surface is polished and is put into electrolytic cell after cleaning；
C, inert gas argon gas is passed through, using sample as anode, platinum electrode is negative electrode, control electric current density 15mA/cm2, constant current
It is electrolysed 15h；Electrolysis temperature is 1 DEG C；
D, above-mentioned electrolyte is filtered with absolute ethyl alcohol after be put into vacuum separation filter and separate precipitate, obtain carbon
Nitride NbC, NbN and M23C6, wherein, described vacuum separation filter is using polycarbonate membrane as filtration supports.
Embodiment two：
The method that the electrolysis of the present invention extracts carbonitride, comprises the following steps：
A, organic electrolyte is added in a cell；The proportioning of the electrolyte is in percentage by weight：Tetramethyl chlorination
Ammonium 2.8%, acetylacetone,2,4-pentanedione 12%, lithium chloride 4%, surplus is 96% methanol；
B, specimen surface is polished and is put into electrolytic cell after cleaning；
C, inert gas argon gas is passed through, using sample as anode, platinum electrode is negative electrode, control electric current density 16mA/cm2, constant current
It is electrolysed 17h；Electrolysis temperature is 2 DEG C；
D, above-mentioned electrolyte is filtered with absolute ethyl alcohol after be put into vacuum separation filter and separate precipitate, obtain carbon
Nitride NbC, NbN and M23C6, wherein, described vacuum separation filter is using polycarbonate membrane as filtration supports.
Embodiment three：
The method that the electrolysis of the present invention extracts carbonitride, comprises the following steps：
A, organic electrolyte is added in a cell；The proportioning of the electrolyte is in percentage by weight：Tetramethyl chlorination
Ammonium 3%, acetylacetone,2,4-pentanedione 13%, lithium chloride 5%, surplus is 98% methanol；
B, specimen surface is polished and is put into electrolytic cell after cleaning；
C, inert gas argon gas is passed through, using sample as anode, platinum electrode is negative electrode, control electric current density 18mA/cm2, constant current
It is electrolysed 18h；Electrolysis temperature is 3 DEG C；
D, above-mentioned electrolyte is filtered with absolute ethyl alcohol after be put into vacuum separation filter and separate precipitate, obtain carbon
Nitride NbC, NbN and M23C6, wherein, described vacuum separation filter is using polycarbonate membrane as filtration supports.
Claims (3)
1. a kind of method that electrolysis extracts carbonitride, it is characterised in that comprise the following steps：
A, organic electrolyte is added in a cell；The proportioning of the electrolyte is in percentage by weight：Tetramethyl chlorination
Ammonium 2.5~3%, acetylacetone,2,4-pentanedione 10~13%, lithium chloride 3~5%, surplus is 95~98% methanol；
B, specimen surface is polished and is put into electrolytic cell after cleaning；
C, inert gas is passed through, using sample as anode, platinum electrode is negative electrode, control electric current 15~18mA/cm2 of density, constant current
It is electrolysed 15~18h；Electrolysis temperature is 1~3 DEG C；
D, above-mentioned electrolyte is filtered with absolute ethyl alcohol after be put into vacuum separation filter and separate precipitate, obtain carbon
Nitride NbC, NbN and M23C6.
2. the method for carbonitride is extracted according to the electrolysis described in claim 1, it is characterised in that：The inert gas is argon
Gas.
3. the method for carbonitride is extracted according to the electrolysis described in claim 1, it is characterised in that：The vacuum separation filtering
Device is using polycarbonate membrane as filtration supports.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710137493.7A CN106969965A (en) | 2017-03-09 | 2017-03-09 | A kind of method that electrolysis extracts carbonitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710137493.7A CN106969965A (en) | 2017-03-09 | 2017-03-09 | A kind of method that electrolysis extracts carbonitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106969965A true CN106969965A (en) | 2017-07-21 |
Family
ID=59328420
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710137493.7A Pending CN106969965A (en) | 2017-03-09 | 2017-03-09 | A kind of method that electrolysis extracts carbonitride |
Country Status (1)
| Country | Link |
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| CN (1) | CN106969965A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107505176A (en) * | 2017-07-31 | 2017-12-22 | 北京矿冶研究总院 | Method for extracting and separating nano-scale precipitate in steel by adopting organic electrolyte |
| CN108871924A (en) * | 2018-07-04 | 2018-11-23 | 湖南大学 | A method of extracting carbide from rich chromium cast iron |
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|---|---|---|---|---|
| CN101074907A (en) * | 2007-03-29 | 2007-11-21 | 上海大学 | Method for extracting steel superfine varia by electrolysis method |
| CN101688857A (en) * | 2007-06-29 | 2010-03-31 | 杰富意钢铁株式会社 | Method for analysis of metal sample |
| CN102033008A (en) * | 2010-10-25 | 2011-04-27 | 上海大学 | Method for extracting S30432 steel carbonitride with electrolytic method |
| CN102213654A (en) * | 2011-05-13 | 2011-10-12 | 江阴兴澄特种钢铁有限公司 | Electrolytic extraction and detection method of nonmetallic inclusion in steel by utilizing organic solution |
| CN102818723A (en) * | 2012-09-07 | 2012-12-12 | 首钢总公司 | Method of electrolytically extracting and detecting fine inclusions in steel |
-
2017
- 2017-03-09 CN CN201710137493.7A patent/CN106969965A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| CN101074907A (en) * | 2007-03-29 | 2007-11-21 | 上海大学 | Method for extracting steel superfine varia by electrolysis method |
| CN101688857A (en) * | 2007-06-29 | 2010-03-31 | 杰富意钢铁株式会社 | Method for analysis of metal sample |
| CN102033008A (en) * | 2010-10-25 | 2011-04-27 | 上海大学 | Method for extracting S30432 steel carbonitride with electrolytic method |
| CN102213654A (en) * | 2011-05-13 | 2011-10-12 | 江阴兴澄特种钢铁有限公司 | Electrolytic extraction and detection method of nonmetallic inclusion in steel by utilizing organic solution |
| CN102818723A (en) * | 2012-09-07 | 2012-12-12 | 首钢总公司 | Method of electrolytically extracting and detecting fine inclusions in steel |
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| Title |
|---|
| 冶金部分析情报网: "《日本钢铁工业高速发展的一个重要因素 介绍 日本钢铁分析技术 第2册》", 30 September 1984, 冶金部分析情报网 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107505176A (en) * | 2017-07-31 | 2017-12-22 | 北京矿冶研究总院 | Method for extracting and separating nano-scale precipitate in steel by adopting organic electrolyte |
| CN108871924A (en) * | 2018-07-04 | 2018-11-23 | 湖南大学 | A method of extracting carbide from rich chromium cast iron |
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Application publication date: 20170721 |
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