CN1621819A - Development liquid used for defects detection and preparation method thereof - Google Patents
Development liquid used for defects detection and preparation method thereof Download PDFInfo
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- CN1621819A CN1621819A CN 200410093206 CN200410093206A CN1621819A CN 1621819 A CN1621819 A CN 1621819A CN 200410093206 CN200410093206 CN 200410093206 CN 200410093206 A CN200410093206 A CN 200410093206A CN 1621819 A CN1621819 A CN 1621819A
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Abstract
The present invention is one kind of fault detecting developer liquid and its preparation process. The developer liquid consists of methyl formate, methyl ethyl ketone, methyl cyclohexane, propyl alcohol, cellulose solution, silica, titanic anhydride and zinc oxide powder. Its preparation process includes the steps of sorting material, compounding, dissolving, purifying, inspecting, etc. The developer liquid has low harmful element content and no chelating on nickel-base stainless steel, and is especially suitable for non-destructive fault detection in LPG engineering and nuclear power engineering with high detection sensitivity and great width/depth ratio.
Description
Technical field
The present invention relates to the surface of the work permeation flaw detection, particularly a kind of development liquid used for defects detection and preparation method thereof.
Background technology
The penetrating inspection method has become a kind of important means that is used for detecting the surface of the work microscopic checks in the commercial production since 1934 begin development.The technology of relevant this detection method, equipment etc. have had more research, but this infiltration detection meeting stays any sequelae to workpiece, still after development of special petrochemical complex and Nuclear Power Engineering, those detect and are judged to qualified surface of the work through the penetrating inspection method, because of residual flaw detection agent (comprising penetrating fluid, imaging liquid, cleaning fluid) arranged, in running in the future, cause burn into to cause leakage, bring out serious accident, just attract much attention.
Discover have several elements can cause some needle-like burn into grain boundary attack of metal material, particularly stainless steel surfaces etc. in the bleeding agent.As just announced three kinds of harmful elements in nuclear engineering file (for example HAF file), they are: fluorine, chlorine, sulphur.Their free state and the content of chemical combination attitude are all wanted strict control.For example: French RCC-M-F6423 standard code, the content of fluorine, chlorine, sulphur all must not surpass 200PPm in the penetrant flaw detection agent, Chinese Industrial Standards (CIS) Q/UCAB005-1999[B3100 (1999) 3031] middle regulation, the content of chlorine is no more than 100PPm, and the content of fluorine, sulphur is no more than 50PPm.
In the nuclear industry, the metal material majority of vitals can be subjected to high temperature, high pressure, high flux radiation.Work after the match and the metal material in liquefied natural gas (LNG) (LNG, the CNG) engineering is in high pressure, utmost point low temperature, alterante stress, environment is more abominable.At this moment, the brittle fracture under low temperature of metal (the particularly inner bag that directly contacts with liquefied natural gas (LNG)) is than whenever all responsive.In the penetrant flaw detection agent harmful element except that with Nuclear Power Engineering in have the identical ill-effect, cause the harmfulness of brittle fracture under low temperature in addition.Especially for cargo ships such as liquified natural gas carrier (LNGC) or liquid chlorine, liquid Celfume, sulphuric dioxide, oxirane, because of its liquid goods that transports is greatly to the harm of environment, must strict supervision.According to " International Code for the Construction and Equipment of Ships Carrying Liquefied Gases in Bulk " is IGC rule (International Codefor the Construction-and Equipment of Ships Carrying Liquefied Gases inBuIk) regulation, and the material of delivery vehicle can not cause accidents such as explosion, burning with liquid goods generation burn into low-temperature embrittleness, high-temerature creep, high pressure surrender etc.But,, can directly form or impel indirectly the Fundamentals that form burn into embrittlement, creep just to some contained harmful elements in the used flaw detection agent of the stainless steel material flaw detection of this class delivery vehicle.So the content that harmful element in the penetrant flaw detection agent that uses in the construction of instrument is carried in strict this class liquid shipping of control can not be ignored.
Experimental study and practice are investigated and to be shown, bring out harmful element that metal such as this class stainless steel destroys except fluorine, chlorine, sulphur, also have sodium, phosphorus (document: Resch G; Odenthal, H:Korrosion 15, Weinheim; Verlag Chemie 1992, S, 33; H.Kaesche:Die Korrosion der Metalle.Zweite Vollig neubearbeitete und erweiterte Auflage Springer-Verlag Berlin, Heidelberg.New York 1979; Fracture of brittle Solids B.R.Lawn T.R.Wilshaw, Cambridge University Press).Special in the stainless steel material that is under the loaded-up condition, normal temperature is during to low temperature (below 20 ℃) state, and except the influence of fluorine, chlorine, sulphur, sodium and phosphorus are also bigger to its destruction.Sodion easily and halogen do not have element and be combined into salt, NaCl for example, this class material impels the metal surface to form serious pitting.The sodion of free state also is one of key factor that forms grain boundary attack.Phosphonium ion can play great facilitation in hot-short, cold short.And the liquid shipping is carried the working temperature of instrument (as the LNG ship) and can be reached-163 ℃, is significantly less than-20 ℃, and visible environment is more abominable, and the possibility that embrittlement takes place is bigger.Therefore, shipping is carried instrument especially as liquefied natural gas (LNG) (LNG, CNG) engineering penetrant flaw detection agent for liquid, except that the content of wanting strict control fluorine, chlorine, three kinds of harmful elements of sulphur, also must strictly control the content of sodium, P elements.But, up to the present, also do not have such penetrant flaw detection agent (penetrating fluid, imaging liquid, cleaning fluid) and control criterion thereof to come out.Domestic once had a penetrant flaw detection agent patent, CN87101195 for example, but it did not make interpellation for objectionable impurities.(ASTM D129-95, ASME: sulphur was had restriction American Society of Mechanical Engineers (AMSE)), ASME-SD-808 (ASTM D80895) had restriction to chlorine to external ASME-SD-129.The currently used penetrant flaw detection agent overwhelming majority does not add control to harmful element fluorine, chlorine, sulphur, have only only a few (for example ship board nuclear level stain penetrant flaw detection agent) that fluorine, chlorine, sulphur are had control, and for important harmful element sodium, the control of phosphorus, also find no so far and close report.
In addition, as a kind of main material of making defeated instrument of liquid shipping or packing, Ni-based stainless steel (for example invar (36% nickel steel)) with all can produce serious chelation after existing various penetrant flaw detection agents contact, its surface is touched regional variable color blackout, to be that its nickel-base alloy surface has embedded nonmetal-and mainly be hydrocarbon and their derivative, weakened the antirust ability of nickel-base alloy, between chelating layer and inner layer metal, all can produce " primary element " phenomenon on the separatrix in chelating district and non-chelating district, cause corrosion of metal, under low temperature environment, reduce Ni-based stainless toughness, destroy croop property and make it produce embrittlement, make liquid shipping security defeated and storage be on the hazard.
Summary of the invention
The object of the present invention is to provide a kind of development liquid used for defects detection and preparation method thereof, have harmful element content height such as fluorine, chlorine, sulphur, sodium, phosphorus in the flaw detection imaging liquid now to solve, and existing flaw detection imaging liquid contacts the problem of the serious chelation of meeting generation with Ni-based stainless steel.
The total design of the present invention is to adopt dipole film dialysis technology, macropore ion exchange resin adsorption technology, the organic solvent of opposed polarity, oxide to be mixed with a kind of fluorine, chlorine, sulphur, sodium, development liquid used for defects detection that phosphorus element content is low, to adapt to the requirement of Ni-based stainless steel engineerings such as Nuclear Power Engineering and liquefied natural gas (LNG) engineering to the imaging liquid of detecting a flaw.
For achieving the above object, the invention provides a kind of development liquid used for defects detection, its raw material is composed as follows:
Sequence number raw material weight number percent (%)
1. formic acid-methyl esters 10～68
2. MEK 8～15
3. methylcyclohexane 6～30
4. propyl alcohol 10～15
5. cellulose solution 4～18
6. monox 1～4
7. titanium does 2～4
8. Zinc Oxide 1～4.
The present invention also provides the preparation method of above-mentioned development liquid used for defects detection, comprises the following steps:
1. screen raw material: the harmful element fluorine in each raw material, chlorine, sulphur, sodium, phosphorus all are no more than 1200PPm and can use;
2. raw materials weighing: according to above-mentioned recipe calculation and each raw material of weighing;
3. normal-temperature operation drops into successively by the listed raw material order of above-mentioned prescription, since second raw material, after a kind of raw material mixes before treating, can drop into down a kind of raw material, finishes until all raw material inputs;
4. purification processes: adopt qualitative filter, quantitatively filter, dipole membrane filtration, macropore ion exchange resin adsorb to the 3. the solution that obtains of step carry out purification processes;
5. detect: when the chlorine＜95PPm in the solution, fluorine≤45PPm, sulphur≤45PPm, sodium≤100PPm, phosphorus≤100PPm,, otherwise repeat the 4. step purification processes again for qualified.
To purification solution detect qualified after, carry out sensitivity test: the sample of this imaging liquid is tested in the test piece of special-purpose crack with its supporting penetrating fluid, cleaning fluid, determined that it is 0.0001mm that test solution can detect width, breadth depth ratio is 1/10 man-made fracture.
Beneficial effect of the present invention:
1, development liquid used for defects detection provided by the invention because of its Formula Design with and the employing of compound method, reduced the content of fluorine-containing, chlorine, sulphur, sodium, phosphorus harmful element, make the content of following harmful element of monomer in this imaging liquid, free state, chemical combination attitude be controlled to be: chlorinity is no more than 95PPm, fluorine, sulphur are no more than 45PPm, and sodium, phosphorus are no more than 100PPm.Obviously, development liquid used for defects detection provided by the invention removes content with fluorine, chlorine, three kinds of harmful elements of sulphur, and to be controlled at limiting the quantity of of Nuclear Power Engineering standard following, also controlled the content of harmful element sodium, phosphorus, satisfy the needs of defects detection such as current engineering-liquefied natural gas (LNG) of having relatively high expectations (LNG, CNG) engineering metal surface microscopic checks, also be fit to the microscopic checks usefulness that Nuclear Power Engineering detects the metal surface, also be suitable for common engineering certainly and use;
2, development liquid used for defects detection provided by the invention does not play chelation to Ni-based stainless steel, is applicable to the flaw detection usefulness of Ni-based stainless steel engineering (as engineerings such as LNG, nuclear power), and its effect with existing flaw detection imaging liquid is compared as follows table:
| Fluorine | Chlorine | Sulphur | Sodium | Phosphorus | Chelating | |
| RCCM(PPm) | ????200 | ????200 | ????100 | ??- | ??- | Gently |
| ASME(％) | ????1 | ????1 | ????1 | ??- | ??- | Gently |
| Ship board nuclear industry level flaw detection agent (PPm) | ????50 | ????100 | ????50 | ??- | ??- | Heavy |
| Development liquid used for defects detection of the present invention (PPm) | ????45 | ????95 | ????45 | ??40 | ??40 | Do not see |
Annotate: "-" refers to not do interpellation
3, development liquid used for defects detection covering power provided by the invention strong, can with the white suspension reagent of the even adsorbed layer of the moistening formation in multiple metal surface, contain organic pulvis in this development liquid used for defects detection, under the UV-irradiation of common daylight or special use, can form hard contrast with dye penetrant, can't produce variegated, its adsorbed layer is very strong to the adsorptive power of penetrating fluid, and tint retention is arranged, the display trace of microscopic checks forever can be kept; It is applied to the metal surface, can evenly expands, volatilization stays one deck adsorption film then rapidly; Can also solution pervasion liquid at the gel of microscopic checks opening, impel the penetrating fluid in the crack to be drawn to the surface to greatest extent, and expanded, under certain illumination, the microfracture vestige can be high-visible.Development liquid used for defects detection provided by the invention uses together with relevant penetrating fluid and cleaning fluid, its detection sensitivity α height, can reach 0.0001mm, breadth depth ratio η can reach more than 1/10, be higher than general penetrant flaw detection agent (the general penetrant flaw detection agent of Gong Buing in the world, advance the product of Co., Ltd. as Japanese honor, the detection sensitivity that can reach is up to 0.0005mm, and breadth depth ratio is 1/60.Annotate: weigh the height of detection level on the engineering, the α value is the smaller the better, and the η value is the bigger the better).
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1:
The compositing formula of this development liquid used for defects detection is as follows:
Sequence number raw material weight number percent (%)
1. formic acid-methyl esters 68
2. MEK 8
3. methylcyclohexane 6
4. propyl alcohol 10
5. cellulose solution 4
6. monox 1
7. titanium does 2
8. Zinc Oxide 1.
Its preparation method comprises the following steps:
1. screen raw material: the harmful element fluorine in each raw material, chlorine, sulphur, sodium, phosphorus all are no more than 1200PPm and can use;
2. raw materials weighing: according to above-mentioned recipe calculation and each raw material of weighing;
3. normal-temperature operation drops into successively by above-mentioned listed raw material order, since second raw material, after a kind of raw material mixes before treating, can drop into down a kind of raw material, finishes until all raw material inputs;
4. purification processes: adopt qualitative filter, quantitatively filter, dipole membrane filtration, macropore ion exchange resin adsorb to the 3. the solution that obtains of step carry out purification processes;
5. detect: when the chlorine＜95PPm in the solution, fluorine≤45PPm, sulphur≤45PPm, sodium≤100PPm, phosphorus≤100PPm,, otherwise repeat the 4. step purification processes again for qualified;
6. sensitivity test: the sample of this imaging liquid is tested in the test piece of special-purpose crack with its supporting penetrating fluid, cleaning fluid, determined that it is 0.0001mm that test solution can detect width, breadth depth ratio is 1/10 man-made fracture.
Embodiment 2:
The compositing formula of this development liquid used for defects detection is as follows:
Sequence number raw material weight number percent (%)
1. formic acid-methyl esters 10
2. MEK 15
3. methylcyclohexane 30
4. propyl alcohol 15
5. cellulose solution 18
6. monox 4
7. titanium does 4
8. Zinc Oxide 4.
Its preparation method is with embodiment 1.
Embodiment 3:
The compositing formula of this development liquid used for defects detection is as follows:
Sequence number raw material weight number percent (%)
1. formic acid-methyl esters 45
2. MEK 12
3. methylcyclohexane 18
4. propyl alcohol 12
5. cellulose solution 5
6. monox 3
7. titanium does 3
8. Zinc Oxide 2.
Its preparation method is with embodiment 1.
Claims (3)
1, a kind of development liquid used for defects detection is characterized in that its raw material is composed as follows:
Sequence number raw material weight number percent (%)
1. formic acid-methyl esters 10～68
2. MEK 8～15
3. methylcyclohexane 6～30
4. propyl alcohol 10～15
5. cellulose solution 4～18
6. monox 1～4
7. titanium does 2～4
8. Zinc Oxide 1～4.
2, the preparation method of the described development liquid used for defects detection of claim 1 is characterized in that comprising the following steps:
1. screen raw material: the harmful element fluorine in each raw material, chlorine, sulphur, sodium, phosphorus all are no more than 1200PPm and can use;
2. raw materials weighing: according to the described recipe calculation of claim 1 and each raw material of weighing;
3. normal-temperature operation drops into successively by listed raw material order in the claim 1, since second raw material, after a kind of raw material mixes before treating, can drop into down a kind of raw material, finishes until all raw material inputs;
4. purification processes: adopt qualitative filter, quantitatively filter, dipole membrane filtration, macropore ion exchange resin adsorb to the 3. the solution that obtains of step carry out purification processes;
5. detect: when the chlorine＜95PPm in the solution, fluorine≤45PPm, sulphur≤45PPm, sodium≤100PPm, phosphorus≤100PPm,, otherwise repeat the 4. step purification processes again for qualified.
3, preparation method according to claim 2, it is characterized in that to purification solution detect qualified after, carry out sensitivity test: the sample of this imaging liquid is tested in the test piece of special-purpose crack with its supporting penetrating fluid, cleaning fluid, determine that it is 0.0001mm that test solution can detect width, breadth depth ratio is 1/10 man-made fracture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410093206 CN1621819A (en) | 2004-12-17 | 2004-12-17 | Development liquid used for defects detection and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410093206 CN1621819A (en) | 2004-12-17 | 2004-12-17 | Development liquid used for defects detection and preparation method thereof |
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| Publication Number | Publication Date |
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| CN1621819A true CN1621819A (en) | 2005-06-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443888C (en) * | 2006-11-17 | 2008-12-17 | 二重集团（德阳）重型装备股份有限公司 | Water based anticorrosive penetrant inspection agent, and preparation method |
| CN101055258B (en) * | 2007-04-29 | 2010-12-08 | 中国船舶重工集团公司第十二研究所 | Hydraulic pressure welding seam leak-checking agent and preparation method thereof |
| CN102205471A (en) * | 2011-05-23 | 2011-10-05 | 太原钢铁(集团)有限公司 | Splash-preventing agent and preparation method thereof |
| CN104614382A (en) * | 2015-01-23 | 2015-05-13 | 苏州新美达探伤器材有限公司 | Environment-friendly imaging agent for liquid penetrant test and preparation method for imaging agent |
-
2004
- 2004-12-17 CN CN 200410093206 patent/CN1621819A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443888C (en) * | 2006-11-17 | 2008-12-17 | 二重集团（德阳）重型装备股份有限公司 | Water based anticorrosive penetrant inspection agent, and preparation method |
| CN101055258B (en) * | 2007-04-29 | 2010-12-08 | 中国船舶重工集团公司第十二研究所 | Hydraulic pressure welding seam leak-checking agent and preparation method thereof |
| CN102205471A (en) * | 2011-05-23 | 2011-10-05 | 太原钢铁(集团)有限公司 | Splash-preventing agent and preparation method thereof |
| CN104614382A (en) * | 2015-01-23 | 2015-05-13 | 苏州新美达探伤器材有限公司 | Environment-friendly imaging agent for liquid penetrant test and preparation method for imaging agent |
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