CN102321840B - Method for preparing hydrogen sulphide stress cracking-resistant steel based on current carrier control technology - Google Patents
Method for preparing hydrogen sulphide stress cracking-resistant steel based on current carrier control technology Download PDFInfo
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- CN102321840B CN102321840B CN 201110307792 CN201110307792A CN102321840B CN 102321840 B CN102321840 B CN 102321840B CN 201110307792 CN201110307792 CN 201110307792 CN 201110307792 A CN201110307792 A CN 201110307792A CN 102321840 B CN102321840 B CN 102321840B
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Abstract
The invention relates to a method for preparing hydrogen sulphide stress cracking-resistant steel based on a current carrier control technology. The method comprises the following steps of: (1) mixing 1.0g of nano Nb, 1.0g of nano B, 0.5 to 1.5g of nano V, 0.5 to 1.5g of nano Cu, 0.5 to 1.0g of nano Mn and 0.5 to 1.0g of rare earth scandium to obtain nano mixed powder; and (2) mixing the nano mixed powder and 100g of steel, smelting, casting to obtain slab, and further processing the slab to obtain the hydrogen sulphide stress cracking-resistant steel. The hydrogen sulphide stress cracking-resistant steel is prepared by utilizing a relationship between current carrier density and the hydrogen sulphide stress cracking resistance of the steel; the preparation method is simple, and low in cost, has not high requirement on equipment and is suitable for mass production; and the steel has high hydrogen sulphide stress cracking resistance.
Description
Technical field
The invention belongs to the preparation field of anti-H 2 S stress cracking steel, particularly a kind of method for preparing anti-H 2 S stress cracking steel based on carrier control technique.
Background technology
Contained H in China's oil and the Sweet natural gas
2S concentration is higher, in recent years, along with oil and natural gas output improves constantly, wet H
2Cause the H of pressurized vessel and pipeline under the S environment
2S stress corrosion accidents such as (SSC) has the trend of continuous rising, at H
2In the pipeline damage that the S corrosion causes, H
2Therefore S stress corrosion cracking (to call SSCC in the following text) accounts for very big ratio, and the destruction of causing is also bigger, to the anti-H of pipeline
2The S corrosive nature is had higher requirement.Be security and the normal operation of guaranteeing steel, carry out the anti-H of steel
2The research of S corrosive nature is very necessary.
The mechanism that sulfide-stress cracking (SSCC) produces is the inside that the Wasserstoffatoms of hydrogen sulfide generation is penetrated into steel, is dissolved in the lattice, causes fragility, is adding formation cracking under tensile stress or the unrelieved stress effect.So SSCC betides the high firmness district of weld seam and heat affected zone usually.
At present domestic and international many investigators have carried out a large amount of research to aspects such as the anti-SSCC performance of steel, SSCC influence factor, SSCC mechanism of corrosion, still, and from the angle of current carrier effect but seldom to the research of the hydrogen sulfide stress crack corrosion of steel.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method for preparing anti-H 2 S stress cracking steel based on carrier control technique; This method has utilized the relation between carrier density and the anti-SSCC performance of steel to prepare anti-SSCC stress cracking steel; This preparation method is simple; Cost is relatively low, and less demanding to equipment is fit to large-scale production; The anti-SSCC stress cracking performance of the steel of gained is high.
Of the present inventionly a kind ofly prepare the method for anti-H 2 S stress cracking steel, comprising based on carrier control technique:
(1) preparation of nano mixed powder: nanometer Nb1.0g, nanometer B1.0g, nanometer V0.5-1.5 g, nanometer Cu0.5-1.5 g, nanometer Mn0.5-1.0g and rare earth scandium Sc0.5-1.0g are mixed, get the nanometer mixed powder;
(2) with above-mentioned nanometer mixed powder with after the 100g steel mix, carry out melting, casting obtains slab; At last the gained slab is further processed, promptly got anti-H 2 S stress cracking steel.
The quality of the nanometer Nb described in the step (1), nanometer B, nanometer V, nanometer Cu, nanometer Mn and rare earth scandium is respectively 1.0g, 1.0g, 0.5g, 0.5g, 0.5g and 0.5g.
The quality of the nanometer Nb described in the step (1), nanometer B, nanometer V, nanometer Cu, nanometer Mn and rare earth scandium is respectively 1.0g, 1.0g, 1.0g, 1.0g, 0.5g and 0.5g.
The quality of the nanometer Nb described in the step (1), nanometer B, nanometer V, nanometer Cu, nanometer Mn and rare earth scandium is respectively 1.0g, 1.0g, 1.0g, 1.0g, 1.0g and 1.0g.
The quality of the nanometer Nb described in the step (1), nanometer B, nanometer V, nanometer Cu, nanometer Mn and rare earth scandium is respectively 1.0g, 1.0g, 1.5g, 1.5g, 1.0g and 1.0g.
Steel described in the step (2) are X70 series pipe line steel, L245 series steel plate or No. 45 steel.
The used steel of step (2) pass through pre-treatment in advance, and treatment process is: earlier steel are carried out electrochemical deoiling, carry out ultrasonic heat washing, UW cold wash, the washing of weak burn into ultrasonic heat and UW cold wash then successively, get heavy and dry at last.
In the melting described in the step (2), smelting temperature is 1550-1600 ℃, and smelting time is 40-50min.
Melting described in the step (2) is for carrying out melting in medium frequency induction melting furnace.
Above-mentioned medium frequency induction melting furnace is antivacuum medium frequency induction melting furnace.
The gained slab is further processed described in the step (2), its technology is: at 1200 ℃ of following austenitizings, it is 1100 ℃ that the beginning is rolled temperature with described slab, and finishing temperature is 850 ℃; Rolling the fast cold beginning temperature in back is 800 ℃, 550 ℃ of fast cold final temperatures; The surface cool speed control of slab is 1 ℃ of-15 ℃/S.
The present invention uses carrier control technique, and the relation between carrier density and the steel plate anti-H 2 S stress cracking performance is furtherd investigate, and the concrete operations step is following:
(1) No. 45 steel are carried out pre-treatment, its technical process is: earlier steel is carried out electrochemical deoiling, carry out ultrasonic heat washing, UW cold wash, the washing of weak burn into ultrasonic heat and UW cold wash then successively, get heavy and dry at last;
(2) preparation of nano mixed powder:
Nanometer Nb, nanometer B, nanometer V, nanometer Cu, nanometer Mn, rare earth scandium (Sc) are weighed up 4 groups of ratio samples in different mass respectively, put into dry wide mouth cup and mix, promptly obtain 4 groups of nanometer mixed powders; Wherein the quality of nanometer Nb, nanometer B, nanometer V, nanometer Cu, nanometer Mn and rare earth scandium is respectively 1.0g, 1.0g, 0.5g, 0.5g, 0.5g, 0.5g in 4 groups of nanometer mixed powders; 1.0g, 1.0g, 1.0g, 1.0g, 0.5g, 0.5g; 1.0g, 1.0g, 1.0g, 1.0g, 1.0g, 1.0g; 1.0g, 1.0g, 1.5g, 1.5g, 1.0g, 1.0g, number 1,2,3 and 4 respectively;
(3) No. 45 steel that 4 groups of above-mentioned nanometer mixed powders obtained with 100g step (1) are respectively put into antivacuum medium frequency induction melting furnace and are carried out non-vacuum melting; 1600 ℃ of smelting temperatures; Smelting time 50min, casting obtains 4 kinds of slabs (modification slab 1, modification slab 2, modification slab 3 and modification slab 4) respectively then;
(4) No. 45 steel that 100g step (1) obtained are put into antivacuum medium frequency induction melting furnace and are carried out non-vacuum melting, 1600 ℃ of smelting temperatures, smelting time 50min, cast then unmodified slab;
(5) be at 1200 ℃ of following austenitizings with step (3) and (4) resulting slab difference processing parameter, it is 1100 ℃ that the beginning is rolled temperature, and finishing temperature is 850 ℃; Rolling the fast cold beginning temperature in back is 800 ℃, 550 ℃ of fast cold final temperatures; The surface cool speed control of modification slab 1, modification slab 2, modification slab 3, modification slab 4 and unmodified slab is 1 ℃/S, 5 ℃/S, 10 ℃/S, 15 ℃/S and 20 ℃/S.
(6) the steel plate line after rolling cuts out the fritter of 10mm * 10mm size with step (5) respectively, is used for doing the current carrier test; Another major part is done stress corrosion dehiscence resistant (SSCC) experiment.
The test of carrier density, its concrete steps are following:
(1) is the test electrode base material with the pat, behind epoxy sealing, gets one of them flat surface as workplace; Adopt thin abrasive paper for metallograph polishing, after absolute ethyl alcohol, acetone clean successively, drying; Promptly get test electrode, be positioned over test electrode in the moisture eliminator subsequent use.
(2) electrode to be measured is soaked into the 10%Na by AR and deionized water preparation
2SO
4Solution is reference electrode with the SCE, and platinum electrode is a supporting electrode, on the CHI660C electrochemical workstation of computer control, carries out current potential-capacity measurement, then data is drawn the Mott-Schottky analysis, and according to the Mott-Schottky relational expression:
The P type:
The N type:
Wherein, Csc is a space charge layer capacitance, and ε is the specific inductivity (19.547 * 10 of organic-containing materials
-13F/m), ε
0For permittivity of vacuum (is 8.854 * 10
-12F/m), e is an electron charge, N
DBe carrier density, U is an externally-applied potential, U
FbBe flat-band potential, k is a Boltzmann constant, and T is a T; Therefore, can obtain modification steel plate carrier density N by the straight-line segment slope of Mott-Schottky analysis
D
Carrier concentration before and after the modification of table 1 steel plate
The test of anti-H 2 S stress cracking, concrete grammar is following:
Carry out tension test according to NACE TM0177-2005 standard A method standard, purity nitrogen, hydrogen sulfide are used in test, adopt the analytical pure chemical reagent, and solution is the sodium-chlor (sodium-chlor of 50g) that contains 5.0wt% and the Glacial acetic acid min. 99.5 (CH of 5.0g of 0.5wt%
3COOH) zero(ppm) water; Test is carried out 720h according to standard, and the loading ratio is 90% SMYS of material, and the speed feeding hydrogen sulfide with 100mL/min begins behind the 1h to clock R
T0.5Interior temperature is controlled between 25 ± 2 ℃, is no more than 4.0 during the off-test of control pH value of solution value.
Table 25 kind of sample anti-H 2 S stress cracking test-results
Can know that by the result along with the rising of carrier concentration, steel plate anti-H 2 S stress cracking performance also promotes thereupon.
The present invention uses carrier control technique, and the relation between carrier density and the steel plate anti-H 2 S stress cracking performance is furtherd investigate.In view of main anti-H 2 S stress cracking research now concentrate on X70 series pipe line steel, above the L245 series steel plate, and in order to make test effect obvious further, the present invention selects for use commercially available No. 45 steel as the test steel, carries out the modification of anti-H 2 S stress cracking.
The present invention is through calculating the carrier density of modification steel, and measures the anti-SSCC performance of steel plate simultaneously, thereby draws the carrier density of modification steel and the corresponding relation between the anti-SSCC stress cracking.The result shows, along with the rising of the carrier concentration order of magnitude, anti-SSCC stress also is improved thereupon in No. 45 steel plates.Carrier concentration increases about 2 one magnitude, and anti-SSCC performance can bigger to some extent accordingly improve.Hence one can see that, can significantly improve steel anti-H 2 S stress cracking performance No. 45 through carrier control technique.
Different and different rolling speed of cooling prepares four groups of modification steel plates with the content of nano-powder Nb, B, V, Cu, Mn, rare earth scandium (Sc), carries out performance comparison with unmodified steel plate.Discover that along with the rising of the carrier concentration order of magnitude in the steel, steel anti-H 2 S stress cracking performance also improves thereupon, hydrogen sulfide stress cracking phenomenon no longer appears in steel plate.
Beneficial effect
(1) the present invention has utilized the relation between carrier density and No. 45 anti-SSCC performances of steel to prepare anti-SSCC stress cracking steel, and this preparation method is simple, and cost is relatively low, and less demanding to equipment is fit to large-scale production;
(2) the stress corrosion dehiscence resistant steel stress-corrosion-cracking resistance of gained of the present invention is high.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
100g 45 tempering are learned oil removing → ultrasonic heat washing → UW cold wash → weak corrosion → ultrasonic heat washing → UW cold wash → get weight → oven drying; Put into antivacuum medium frequency induction melting furnace; Interpolation 1.0g nanometer Nb, 1.0g nanometer B, 0.5g nanometer V, 0.5g nanometer Cu, 0.5g nanometer Mn, 0.5g rare earth scandium (Sc) carry out non-vacuum melting; 1600 ℃ of smelting temperatures, smelting time 50min, casting obtains slab.
With slab controlled rolling processing parameter is at 1200 ℃ of following austenitizings, and it is 1100 ℃ that the beginning is rolled temperature, and finishing temperature is 850 ℃.Rolling the fast cold beginning temperature in back is 800 ℃, 550 ℃ of fast cold final temperatures, and the surface cool speed control is 1 ℃/S.Obtain the Mott-Schottky analysis of sample electrode to be measured then, obtain modification steel carrier density N
D-1, see table 3.Carry out tension test according to NACE TM0177-2005 standard A method standard at last, sample is carried out the anti-H 2 S stress cracking performance detect, see table 4.
Embodiment 2
100g 45 tempering are learned oil removing → ultrasonic heat washing → UW cold wash → weak corrosion → ultrasonic heat washing → UW cold wash → get weight → oven drying; Put into antivacuum medium frequency induction melting furnace; Interpolation 1.0g nanometer Nb, 1.0g nanometer B, 1.0g nanometer V, 1.0g nanometer Cu, 0.5g nanometer Mn, 0.5g rare earth scandium (Sc) carry out non-vacuum melting; 1550 ℃ of smelting temperatures, smelting time 50min, casting obtains slab.
With slab controlled rolling processing parameter is at 1200 ℃ of following austenitizings, and it is 1100 ℃ that the beginning is rolled temperature, and finishing temperature is 850 ℃.Rolling the fast cold beginning temperature in back is 800 ℃, 550 ℃ of fast cold final temperatures, and the surface cool speed control is 5 ℃/S.Obtain the Mott-Schottky analysis of sample electrode to be measured then, obtain modification steel carrier density N
D-2, see table 3.Carry out tension test according to NACE TM0177-2005 standard A method standard at last, sample is carried out the anti-H 2 S stress cracking performance detect, see table 4.
Embodiment 3
The 100g45 tempering is learned oil removing → ultrasonic heat washing → UW cold wash → weak corrosion → ultrasonic heat washing → UW cold wash → get weight → oven drying; Put into antivacuum medium frequency induction melting furnace; Interpolation 1.0g nanometer Nb, 1.0g nanometer B, 1.0g nanometer V, 1.0 nanometer Cu, 1.0g nanometer Mn, 1.0g rare earth scandium (Sc) carry out non-vacuum melting; 1580 ℃ of smelting temperatures, smelting time 45min, casting obtains slab.
With slab controlled rolling processing parameter is at 1200 ℃ of following austenitizings, and it is 1100 ℃ that the beginning is rolled temperature, and finishing temperature is 850 ℃.Rolling the fast cold beginning temperature in back is 800 ℃, 550 ℃ of fast cold final temperatures, and the surface cool speed control is 10 ℃/S.Obtain the Mott-Schottky analysis of sample electrode to be measured then, obtain modification steel carrier density N
D-3, see table 3.Carry out tension test according to NACE TM0177-2005 standard A method standard at last, sample is carried out the anti-H 2 S stress cracking performance detect, see table 4.
Embodiment 4
The 100g45 tempering is learned oil removing → ultrasonic heat washing → UW cold wash → weak corrosion → ultrasonic heat washing → UW cold wash → get weight → oven drying; Put into antivacuum medium frequency induction melting furnace; Interpolation 1.0g nanometer Nb, 1.0g nanometer B, 1.5g nanometer V, 1.5g nanometer Cu, 1.0g nanometer Mn, 1.0g rare earth scandium (Sc) carry out non-vacuum melting; 1600 ℃ of smelting temperatures, smelting time 50min, casting obtains slab.
With slab controlled rolling processing parameter is at 1200 ℃ of following austenitizings, and it is 1100 ℃ that the beginning is rolled temperature, and finishing temperature is 850 ℃.Rolling the fast cold beginning temperature in back is 800 ℃, 550 ℃ of fast cold final temperatures, and the surface cool speed control is 15 ℃/S.Obtain the Mott-Schottky analysis of sample electrode to be measured then, obtain modification steel carrier density N
D-4, see table 3.Carry out tension test according to NACE TM0177-2005 standard A method standard at last, sample is carried out the anti-H 2 S stress cracking performance detect, see table 4.
Carrier concentration before and after the modification of table 3 steel plate
5 kinds of sample anti-H 2 Ss of table 4 stress cracking test-results
Claims (6)
1. one kind prepares the method for anti-H 2 S stress cracking steel based on carrier control technique, comprising:
(1) nanometer Nb 1.0g, nanometer B 1.0g, nanometer V 0.5-1.5g, nanometer Cu 0.5-1.5g, nanometer Mn 0.5-1.0g and rare earth scandium 0.5-1.0g are mixed, get the nanometer mixed powder;
(2) with above-mentioned nanometer mixed powder with after the 100g steel mix, be 1550-1600 ℃ in temperature, the time is under the 40-50min, carries out melting, casting obtains slab; At last the gained slab is further processed, promptly got anti-H 2 S stress cracking steel;
The gained slab is further processed described in the step (2), its technology is: at 1200 ℃ of following austenitizings, it is 1100 ℃ that the beginning is rolled temperature with described slab, and finishing temperature is 850 ℃; Rolling the fast cold beginning temperature in back is 800 ℃, 550 ℃ of fast cold final temperatures; The surface cool speed control of slab is 1 ℃ of-15 ℃/s.
2. according to claim 1ly a kind ofly prepare the method for anti-H 2 S stress cracking steel based on carrier control technique, it is characterized in that: the quality of the nanometer Nb described in the step (1), nanometer B, nanometer V, nanometer Cu, nanometer Mn and rare earth scandium is respectively 1.0g, 1.0g, 0.5g, 0.5g, 0.5g and 0.5g.
3. according to claim 1ly a kind ofly prepare the method for anti-H 2 S stress cracking steel based on carrier control technique, it is characterized in that: the quality of the nanometer Nb described in the step (1), nanometer B, nanometer V, nanometer Cu, nanometer Mn and rare earth scandium is respectively 1.0g, 1.0g, 1.0g, 1.0g, 0.5g and 0.5g.
4. according to claim 1ly a kind ofly prepare the method for anti-H 2 S stress cracking steel based on carrier control technique, it is characterized in that: the quality of the nanometer Nb described in the step (1), nanometer B, nanometer V, nanometer Cu, nanometer Mn and rare earth scandium is respectively 1.0g, 1.0g, 1.0g, 1.0g, 1.0g and 1.0g.
5. according to claim 1ly a kind ofly prepare the method for anti-H 2 S stress cracking steel based on carrier control technique, it is characterized in that: the quality of the nanometer Nb described in the step (1), nanometer B, nanometer V, nanometer Cu, nanometer Mn and rare earth scandium is respectively 1.0g, 1.0g, 1.5g, 1.5g, 1.0g and 1.0g.
6. according to claim 1ly a kind ofly prepare the method for anti-H 2 S stress cracking steel based on carrier control technique, it is characterized in that: the melting described in the step (2) is for carrying out melting in medium frequency induction melting furnace; Described medium frequency induction melting furnace is antivacuum medium frequency induction melting furnace.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854547A (en) * | 2004-12-22 | 2006-11-01 | 北京师范大学 | Self-lubricating friction-reducing bearing of multiple ionic mixed injection |
| CN101928885A (en) * | 2009-06-26 | 2010-12-29 | 上海梅山钢铁股份有限公司 | Hydrothion corrosion resistant pipe steel and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH08320312A (en) * | 1995-05-26 | 1996-12-03 | Mitsui Eng & Shipbuild Co Ltd | Determination method of hydrogen sulfide gas by tcd gas chromatograph |
| US7022644B2 (en) * | 2002-02-20 | 2006-04-04 | Engelhard Corporation | Hydrogen sulfide-suppressing catalyst compositions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854547A (en) * | 2004-12-22 | 2006-11-01 | 北京师范大学 | Self-lubricating friction-reducing bearing of multiple ionic mixed injection |
| CN101928885A (en) * | 2009-06-26 | 2010-12-29 | 上海梅山钢铁股份有限公司 | Hydrothion corrosion resistant pipe steel and production method thereof |
Non-Patent Citations (2)
| Title |
|---|
| JP特开平8-320312A 1996.12.03 |
| 王斌 等.合金元素和控制轧制对低合金高强度钢抗硫化氢腐蚀的影响.《腐蚀与防护》.2005,第26卷(第9期),第402-406页. * |
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