CN1444036A - Penetration liquor for inspection and its preparation method - Google Patents

Abstract

The present invention relates to a penetrating liquod for inspection, and is characterized by that its composition contains benzyl alcohol, ethanol monobuttyl ether, ethylene glycol, propanol, DBP, DIBP, RADGLO-JST-10, RADGLO-JST-16, RADGLO-P10 and RADGL0-P16. Its preparation method includes the following steps: screening raw material, preparing material, dissolving raw material, purification and detection. Its harmful element fluorine, chlorine, sulfur and sodium contents are low, specially, it is suitable for nondestructive inspection in liquefied natural gas engineering and nuclear power engineering.

Description

Penetrating fluid of flaw detection and preparation method thereof

Technical field:

The present invention relates to the flaw detection of workpiece or equipment appearance, the penetrating fluid of flaw detection of particularly a kind of low fluorine, chlorine, sulphur, sodium content.

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 at present since developing since 1934.The technology of this detection method, equipment etc. have had more research.After infiltration detects, can stay any sequelae to workpiece, still thing rarely known by the people.Still nobody is engaged in the discussion of this respect at present.

Since the development Nuclear Power Engineering, those after testing and be judged to qualified surface of the work, residual have a flaw detection agent (comprising penetrating fluid, imaging liquid, cleaning fluid), and generation that cause burn into to cause leakage in running in the future, to bring out serious accident just attracts 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.Announced three kinds of harmful elements in the nuclear engineering 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 chlorine, sulphur 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.Different therewith is, the metal material in liquefied natural gas (LNG) (LNG, the CNG) engineering is in high pressure, utmost point low temperature, alterante stress works after the match, and environment is more abominable.At this moment, the brittle fracture under low temperature of metal (the particularly stainless steel inner container that directly contacts with liquefied natural gas (LNG)) is than whenever all responsive.In the dye penetrant inspection 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.So the content of harmful element has become the thing that receives much attention in the penetrant flaw detection agent that strict control LNG, CNG engineering are used.

Experimental study and practice are investigated and are shown that bring out cold short harmful element except fluorine, chlorine, sulphur, sodium also is a kind of harmful element (document: Resch G; Odenthal, H; Korrosion15, Weinheim; Verlag Chemie1992, S, 33; H.Kaesche; Die Korrosion derMetalle Zweite Vollig neubearbeitete und erweiterte AuflageSpringer-Verlag Berlin, Heidelberg, New York 1979; Fracture ofbrittle Solids B.R.Lawn T.R.Wilshaw, Cambridge University Press).Sodion often 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.For this reason,,, except that wanting strict control fluorine, chlorine, sulphur, also must strictly control with in the penetrant flaw detection agent in the liquefied natural gas (LNG) engineering the content of sodium element.But, up to the present, also do not have such penetrant flaw detection agent.Domestic once had a penetrant flaw detection agent patent, CN87101195.6 for example, but do not do explanation for objectionable impurities yet.External ASME-SD-129 (ASTM D129-95) had restriction to sulphur, and ASME-SD-808 (ASTM D80895) had restriction to chlorine.The current domestic used penetrant flaw detection agent overwhelming majority does not add control to harmful element fluorine, chlorine, sulphur, has only only a few that fluorine, chlorine, sulphur are had control, and for the control of important harmful element sodium, also finds no so far and close report.

In addition, the general penetrant flaw detection agent of Gong Buing (entering Co., Ltd. as the Japanese honor) detection sensitivity that can reach is up to 0.0005mm in the world, and breadth depth ratio is 1/60.

Summary of the invention:

The technical problem to be solved in the present invention is to provide a kind of penetrating fluid of flaw detection and preparation method thereof, make fluorine, chlorine, the sulphur of its preparation, the content of sodium all be no more than 100PPm, it not only can satisfy the flaw detection of Nuclear Power Engineering metal surface microscopic checks, also be applicable to the microscopic checks flaw detection of gas engineering metal surface, certain common engineering construction is no problem more, and the flaw detection the minute crack width can reach 0.0001mm, breadth depth ratio reaches 1/10.

Technical solution of the present invention is as follows:

A kind of penetrating fluid of flaw detection is characterized in that this penetrating fluid is made up of following raw materials according:

Sequence number raw material weight %

1. benzyl alcohol 5～55%

2. ethylene glycol monobutyl ether 8～15%

3. glycol 10～18%

4. propyl alcohol 8～18%

⑤DBP 6～16％

⑥DIBP 8～16％

⑦RADGLO-JST-10 1～2％

⑧RADGLO-JST-16 1～2％

⑨RADGLO-P ₁₀ 1.5～4％

⑩RADGLO-P ₁₆ 1.5～4％

Wherein DBP is a n-butyl phthalate, and DIBP is a diisobutyl phthalate, and RADGO-JST-10 is auspicious dagger-axe fluorescence green, and RADGLO-JST-16 is that auspicious dagger-axe fluorescence is bright red, RADGLO-P ₁₀Be auspicious dagger-axe fluorescein, RADGLO-P ₁₆Be auspicious dagger-axe fluorescence bright red.

The also available propylene glycol of described glycol is replaced or part is replaced;

Described DBP can replace or the part replacement with DAP, and wherein DAP is a diallyl phthalate;

Described DIBP can replace or the part replacement with DEP, and wherein DEP is a diethyl phthalate;

The preparation method of penetrating fluid of flaw detection of the present invention comprises the following steps:

1. screen raw material, select technical pure or chemical pure raw material for use, the content of the fluorine in the raw material, chlorine, sulphur, sodium is analyzed, be no more than can using of 1300PPm;

2. raw materials weighing, the raw material compositing formula of penetrating fluid calculates and each raw material of weighing according to the present invention;

3. under normal temperature condition, dissolve raw material, drop into successively,, after a kind of raw material fully dissolves and stirs before treating, drop into a kind of raw material down again, finish until each raw material input since second raw material by above-mentioned listed raw material order;

4. purification processes: by qualitative filter, quantitatively filter, dipole membrane filtration or macropore ion exchange resin adsorption method to the 3. step dissolve uniform solution and carry out purification processes;

5. the poisonous element of solution of purifying is detected, chlorine＜95PPm, fluorine≤45PPm when sulphur≤45PPm, sodium≤100PPm, for qualified, otherwise repeats the 4. step purification processes again;

6. sensitivity test is tested with its supporting imaging liquid, cleaning fluid the sample of this penetrating fluid in the test piece of special-purpose crack, determines that it is 0.0001mm that test solution can detect width, and breadth depth ratio is that 1/10 man-made fracture is qualified.

Technique effect of the present invention:

The present invention hangs down the penetrating fluid of flaw detection of fluorine, chlorine, sulphur, sodium content, the content to fluorine, chlorine, sulphur, sodium of selecting for use of raw material just has certain control, after most critical is the penetrating fluid preparation, adopted strict purification processes technology, the content of guaranteeing the harmful element of monomer, free state, chemical combination attitude in the penetrating fluid is controlled to be: chlorinity is no more than 95PPm, fluorine, sulphur are no more than 45PPm, and sodium is no more than 100PPm.Obviously, in defluorination of the present invention, chlorine, the sulphur three content of harmful element control reached limiting the quantity of of Nuclear Power Engineering standard in the past following outside, also controlled the content of harmful element sodium first.And must control at present the content of sodium on the liquefied natural gas (LNG) engineering.Obviously, the present invention can satisfy the needs that current engineering-liquefied natural gas (LNG) of having relatively high expectations (LNG, CNG) engineering microscopic checks detects construction, also satisfy Nuclear Power Engineering detect the metal surface the needs of microscopic checks, also be suitable for common engineering construction certainly.

Through probationary certificate, the minute crack width that penetrating fluid of flaw detection of the present invention can be surveyed is 0.0001mm, and breadth depth ratio is 1/10.

Embodiment:

The invention will be further described to enumerate following examples below:

Embodiment 1.

The compositing formula of penetrating fluid of flaw detection of the present invention is as follows:

Sequence number raw material weight %

1. benzyl alcohol 55

2. ethylene glycol monobutyl ether 8

3. glycol 10

4. propyl alcohol 8

⑤DBP 6

⑥DIBP 8

⑦RADGLO-JST-10 1

⑧RADGLO-JST-16 1

⑨RADGLO-P ₁₀ 1.5

⑩RADGLO-P ₁₆ 1.5

Its preparation process comprises the following steps:

1. screen raw material, select technical pure or chemical pure raw material for use, the content of the fluorine in the raw material, chlorine, sulphur, sodium is analyzed, be no more than can using of 1300PPm;

2. raw materials weighing, the raw material compositing formula of penetrating fluid calculates and each raw material of weighing according to the present invention;

3. under normal temperature condition, dissolve raw material, drop into successively,, after a kind of raw material fully dissolves and stirs before treating, drop into a kind of raw material down again, finish until each raw material input since second raw material by above-mentioned listed raw material order;

4. purification processes: by qualitative filter, quantitatively filter, dipole membrane filtration or macropore ion exchange resin adsorption method to the 3. step dissolve uniform solution and carry out purification processes;

5. the solution harmful element of purifying is detected, chlorine＜95PPm, fluorine≤45PPm when sulphur≤45PPm, sodium≤100PPm, for qualified, otherwise repeats the 4. purification processes in step again;

6. sensitivity test is tested with its supporting imaging liquid, cleaning fluid the sample of this penetrating fluid in the test piece of special-purpose crack, determines that it is 0.0001mm that test solution can detect width, and breadth depth ratio is that 1/10 man-made fracture is qualified.

Embodiment 2.

This penetrating fluid of flaw detection is made up of following raw materials according:

Sequence number raw material weight %

1. benzyl alcohol 5

2. ethylene glycol monobutyl ether 15

3. glycol 18

4. propyl alcohol 18

⑤DBP 16

⑥DIBP 16

⑦RADGLO-JST-10 2

⑧RADGLO-JST-16 2

⑨RADGLO-P ₁₀ 4

⑩RADGLO-P ₁₆ 4

Its preparation method is with embodiment 1.

Embodiment 3.

This penetrating fluid of flaw detection is made up of following raw materials according:

Sequence number raw material weight %

1. benzyl alcohol 40

2. ethylene glycol monobutyl ether 8

3. glycol 10

4. propyl alcohol 15

⑤DBP 8

⑥DIBP 10

⑦RADGLO-JST-10 1.2

⑧RADGLO-JST-16 1.8

⑨RADGLO-P ₁₀ 3.5

⑩RADGLO-P ₁₆ 2.5

Its preparation method is with embodiment 1.

In addition, in the foregoing description, described glycol can be replaced or the part replacement with propylene glycol, and described DEP can replace with DAP, and described BIBP can replace or partly replace with DEP, and relevant embodiment no longer enumerates explanation hereby.

Claims (5)

1, a kind of penetrating fluid of flaw detection is characterized in that this penetrating fluid is made up of following raw materials according:

Sequence number raw material weight %

1. benzyl alcohol 5～55%

2. ethylene glycol monobutyl ether 8～15%

3. glycol 10～18%

4. propyl alcohol 8～18%

⑤DBP 6～16％

⑥DIBP 8～16％

⑦RADGLO-JST-10 1～2％

⑧RADGLO-JST-16 1～2％

⑨RADGLO-P ₁₀ 1.5～4％

⑩RADGLO-P ₁₆ 1.5～4％

2, penetrating fluid of flaw detection according to claim 1 is characterized in that: the also available propylene glycol of described glycol is replaced or part is replaced.

3, penetrating fluid of flaw detection according to claim 1 is characterized in that: described DBP can replace or the part replacement with DAP.

4, penetrating fluid of flaw detection according to claim 1 is characterized in that: described DIBP can replace or the part replacement with DEP.

5, according to the preparation method of claim 1 or 2 or 3 or 4 described penetrating fluid of flaw detection, it is characterized in that comprising the following steps:

1. screen raw material, select technical pure or chemical pure raw material for use, the content of the fluorine in the raw material, chlorine, sulphur, sodium is analyzed, be no more than can using of 1300PPm;

2. raw materials weighing, the raw material compositing formula of penetrating fluid calculates and each raw material of weighing according to the present invention;

3. under normal temperature condition, dissolve raw material, drop into successively,, after a kind of raw material fully dissolves and stirs before treating, drop into a kind of raw material down again, finish until each raw material input since second raw material by listed raw material order in the claim 1;

4. purification processes: by qualitative filter, quantitatively filter, dipole membrane filtration or macropore ion exchange resin adsorption method to the 3. step dissolve uniform solution and carry out purification processes;

5. the solution harmful element of purifying is tested, chlorine＜95PPm, fluorine≤45PPm when sulphur≤45PPm, sodium≤100PPm, for qualified, otherwise repeats the 4. step purification processes again;

6. sensitivity test is tested with its supporting imaging liquid, cleaning fluid the sample of this penetrating fluid in the test piece of special-purpose crack, determines that it is 0.0001mm that test solution can detect width, and breadth depth ratio is that 1/10 man-made fracture is qualified.