CN101195703B - Couplant for fault detection and method for producing the same - Google Patents
Couplant for fault detection and method for producing the same Download PDFInfo
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- CN101195703B CN101195703B CN2007102015162A CN200710201516A CN101195703B CN 101195703 B CN101195703 B CN 101195703B CN 2007102015162 A CN2007102015162 A CN 2007102015162A CN 200710201516 A CN200710201516 A CN 200710201516A CN 101195703 B CN101195703 B CN 101195703B
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Abstract
The invention relates to organic chemical technical field, in particular to a soluble anti-corrosion couplant for ultrasonic inspection, and a relative preparation method, wherein the couplant contains 0.5-50% soluble preservative, 10-50% carbowax whose weight average molecular weight M is 400-1000, and 5-50% carbowax whose weight average molecular weight M is 2000-10000, or 10-50% polyether (under 40DEG C, 20000-100000mm<2>/s), 0.01-2% non-silicon compound defoamer, paint, and perfumes, and water of left amount. The couplant has good ultrasonic couple property and good anti-scaling anti-corrosion property on metal, particularly on stainless steel surfacing layer.
Description
Technical field
The present invention relates to a kind of couplant for fault detection and preparation method thereof, belong to the organic chemical industry field.
Background technology
All need carry out the non-destructive test(ing)(NDT) detection in numerous industries such as machinofacture, chemical industry, such as ultrasound examination to the weld seam and the overlay cladding of workpiece.Between probe and workpiece surface, gas cloud is arranged; Hyperacoustic reflectivity is almost 100%; Be difficult to inject the purpose that workpiece does not reach flaw detection, therefore, need coat a kind of medium couplant that transmits sound wave at workpiece surface when implementing ultrasound examination in order to guarantee hyperacoustic ideal propagation.
Disclose with water, machine oil, kerosene, glycerine, emulsified olefin, CMC 99.5, sodium-alginate, XPA etc. as the ultrasound examination couplant among existing disclosed technical information and Chinese patent CN1161863A, CN1161863A, the CN1070927A etc.Though these public technologies can satisfy medical and some the metal ultrasound examination of human body to the requirement of couplant, remain some defectives.As the variation that will cause after not taking into full account couplant and the metallic surface contacting; Do not solve some composition in the couplant and will cause the serious corrosion of overlay cladding of steel surface; And the technical field of aforesaid Chinese patent CN1161863A mainly is the detection of human body medical ultrasonic; Though CN1161863A, CN1070927A two China patent can be used for the metal ultrasound examination; But their main purpose all reduces cost, not emphasis and the key point of the corrosion that prevents iron and steel and overlay cladding surface as own technological invention; Can recognize that according to anti-corrosion of metal knowledge in described couplant, to add behind trolamine, the Sodium Benzoate antirust ability of couplant not strong, more can not eliminate the stainless intergranular corrosion of some pair ion.Simultaneously, according to workpiece surface roughness, the relation of couplant between workpiece surface thickness and transmission ultrasonic wave, use these couplants can not obtain the ideal coupling effect on the overlay cladding surface.
In addition, the ultrasound examination of iron and steel also relates to many important other factorses.As being to finish the final inspection carry out in manufacturing processed when non-destructive test(ing)(NDT), or when not having particular requirement, the material that can use one type in MO usually is the mechanical wet goods of N32 as couplant like the trade mark.And when manufacturing processed not end as yet; When also needing thermal treatment that butt welded seam and overlay cladding do to eliminate stress; Just can not use MO; Because the MO that spreads on weld seam and overlay cladding surface is difficult to remove fully, moreover the expense of removing is very expensive, after these residual MO are heated butt welded seam and overlay cladding is produced harm.Plain mineral oil just forms one deck oil film in the metallic surface; It has certain lubricity; The flaw detection probe can be free to slide at weld seam or overlay cladding surface, but not possess antiseptic property, can't prevent the corrosion in the environment damp and hot, that the metallicity pollutent exists of weld seam and overlay cladding.
In order to satisfy the requirement to couplant such as thermal treatment, in carrying out flaw detection, should use non-mineral oil type couplant for fault detection, that is generally adopted at present has chemical paste class materials such as CMC 99.5, polyvinyl alcohol, glycerine.Like the UT couplant that proposes among Chinese patent CN1161863A, CN1038346A, the CN1070927A.The obvious deficiency that these existing non-mineral oil type couplant for fault detection exist is the antiseptic and rustproof poor-performing to iron and steel, and corrosion appears in weld seam after the carrying out flaw detection and overlay cladding surface easily.And contain the composition that makes the surface cause erosion in these couplant for fault detection usually, like hydroxide ion of cl ions, acetate ion, high density etc., like CN1070927A, all there is such problem in CN1161863A; In CN1038346A, also there are the problems such as nitrite that are detrimental to health of using.Therefore these couplant for fault detection are unwell to large chemical equipment especially, like the UT of hydrogenator and nuclear-power reactor cylindrical shell weld seam and overlay cladding.The weld seam and the overlay cladding of this kind equipment all are made up of stainless steel, and halogens such as cl ions are familiar with by people their damaging effect already, are selecting for use couplant for fault detection to take in.In the production scene; The carbon steel dust that is easy to form ferrite pollution can produce corrosive nature to stainless steel; And the carbon steel of polishing built-up welding stainless steel base is necessary production process, and it almost is impossible therefore will eliminating the dust that takes weld seam and overlay cladding surface thus to fully.Use the mineral oil condition similar with removing the surface, rely on the method for cleaning to remove the dust on weld seam and overlay cladding surface, not only need pay quite big cost, but also the workload that costs a lot of money, it can't be removed in actual operating condition sometimes.Therefore, solve that the inevitable requirement of protection product is not only in these corrosion and be to make to produce smooth important measures.Other non-mineral oil type couplant for fault detection, like glycerine (USP Kosher) etc., not only Corrosion Protection is similar with above-mentioned MO, and its other performance such as viscosity etc. are very undesirable with the situation that temperature, moisture content change.The subtle change of temperature, moisture content just causes the bigger variation of thickness, and we know that the reflection wave height of thickness and UT is closely related, and this variation brings the difficulty on the analysis and judgement to carrying out flaw detection, thereby also inapplicable.
In sum; Existing ultrasound examination is with couplant or can not satisfy the product manufacture requirement; Perhaps has the defective on the performance: not good like non-mineral oil type flaw detection couplant antiseptic property; Coupling effect is not good in large-size chemical and nuclear power generating equipment weld seam and overlay cladding ultrasound examination, is difficult to the requirement of satisfying technology and preventing stainless steel intercrystalline corrosion.The new couplant for fault detection of exploitation is badly in need of in this area.
Summary of the invention
One of technical problem to be solved by this invention provides a kind of couplant for fault detection; This couplant for fault detection is that couplant is used in the UT of a kind of water-soluble anti-rust type; Can satisfy non-destructive test(ing)(NDT) well and detect requirement, and remove fully easily UW coupling and antiseptic property.
The present invention solves this technical problem the technical scheme that is adopted: couplant for fault detection of the present invention, and this couplant for fault detection contains by weight percentage:
Polyoxyethylene glycol (weight-average molecular weight M=400～1000) 10%～50%
Polyoxyethylene glycol (weight-average molecular weight M=2000～10000) 5%～50%
Polyethers (20000～100000mm under 40 ℃
2/ s) 10%～50%
Waterborne-type preservation 0.5%～50%
Water is surplus.
Further, couplant for fault detection of the present invention is composed of the following components by weight percentage:
Polyoxyethylene glycol (weight-average molecular weight M=400～1000) 10%～50%
Polyoxyethylene glycol (weight-average molecular weight M=2000～10000) 5%～50%
Polyethers (20000～100000mm under 40 ℃
2/ s) 10%～50%
Waterborne-type preservation 0.5%～50%
Non-silicon type compound skimmer, dyestuff, spices auxiliary agent 0.01%～2%
Water is surplus
Another provides a kind of preparation method of above-mentioned couplant for fault detection technical problem to be solved by this invention.
The present invention solves this technical problem the technical scheme that is adopted: the preparation method of couplant of the present invention comprises the steps:
(1) preparation waterborne-type preservation; A. in the reaction unit that atmospheric condenser and TM are housed, be in molar ratio: lipid acid 0.85～1.05, nitrogenous compound 0.95～1.25; Epoxy compounds 0.15～0.30 adds each raw material; Drip 98% vitriol oil, the control rate of addition, hierarchy of control temperature is within 50 ℃; B. be warming up to 185～195 ℃ after adding, insulation reaction 1.5～2.5 hours, the water that reaction generates is steamed simultaneously; C. cool off above-mentioned reactant, add excessive quicklime, distill distillate and anhydrous sodium sulfate drying; D. filter, filtrating adds an amount of activated carbon, refluxes then 30～50 minutes, and the cut of collecting 150～165 ℃ makes waterborne-type preservation;
(2) the further esterification of waterborne-type preservation: in another reaction unit, add the waterborne-type preservation back log of producing through above-mentioned steps; Be warming up to and add the polyoxyethylene glycol of weight-average molecular weight M=2000～10000 after 50 ± 5 ℃ again and be heated to 120 ℃～140 ℃, fully stirred 25～45 minutes;
(3) add polyoxyethylene glycol (weight-average molecular weight M=400～1000) and polyethers (20000～100000mm under 40 ℃
2/ the viscosity of s) treating product reaches 40 ℃ of 50～150mm down
2Between/the s with acid number less than 0.01 o'clock, stopped reaction;
(4) naturally cooling is added the zero(ppm) water of surplus, makes water-soluble anti-corrosive type couplant for fault detection.
Further technical scheme is in above-mentioned steps (4), and when naturally cooling to below 80 ℃, also the couplant total weight percent by preparation adds 0.01%～2% non-silicon type compound skimmer, dyestuff, spices auxiliary agent.
The invention has the beneficial effects as follows: provide the UT of a kind of water-soluble anti-rust type to use couplant; Couplant of the present invention is water-soluble; It can conveniently be removed by water; Composition attached to weld seam or overlay cladding surface evaporates in the subsequent heat treatment operation or voluntarily, perhaps can not produce harmful product, and couplant of the present invention has anti-corrosion function in the flaw detection process and after the carrying out flaw detection, and it can protect the blue oxide film on overlay cladding surface can not change the brown iron rust into especially.Therefore, couplant of the present invention has crucial meaning for the welding quality manufacturing detection of large-size chemical and nuclear power generating equipment.The preparation method of couplant for fault detection of the present invention, simple to operation, preparation equipment there is not particular requirement.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Couplant for fault detection of the present invention contains: the polyoxyethylene glycol 5%～50% of water miscible sanitas 0.5%～50%, polyoxyethylene glycol (weight-average molecular weight M=400～1000) 10%～80% and weight-average molecular weight M=2000～10000 or polyethers (40 ℃ of 20000～100000mm down by weight percentage
2/ s) 10%～50% etc., wherein: said water miscible sanitas by C6～C12 lipid acid, organic amine, epoxy compounds in the presence of catalyzer at first reaction form waterborne-type preservation and then with the polyoxyethylene glycol generation ester that further reacts;
As preferred embodiment a kind of; Couplant for fault detection of the present invention is composed of the following components by weight percentage: water miscible sanitas 0.5%～50%, the polyoxyethylene glycol 5%～50% of polyoxyethylene glycol (molecular weight 400～1000) 10%～80% and weight-average molecular weight M=2000～10000 or polyethers (20000～100000mm under 40 ℃
2/ s) 10%～50%, non-silicon type compound skimmer, dyestuff, spices auxiliary agent 0.01%～2%, water are surplus.
Wherein, Above-mentioned water miscible sanitas is formed by lipid acid, nitrogenous compound, epoxy compounds and catalyzer prepared in reaction under specified requirements, and the mol ratio of used each material is: lipid acid 0.85～1.05, nitrogenous compound 0.95～1.25, epoxy compounds 0.15～0.3.The carbochain of said lipid acid is C
6～C
18, say that more specifically they can be one or more the compsns in caproic acid, sad, sebacic acid, LAURIC ACID 99 MIN, the oleic acid.Said nitrogenous compound is thanomin, diethylolamine, trolamine, pyridine and verivate thereof etc., and purity should be more than 99%.Said epoxy compounds is oxyethane, propylene oxide, and catalyzer such as 1,4 nitrogen oxygen hexane and verivate thereof are that concentration is 98% sulfuric acid, and its consumption shows acidity degree of being with the system of being controlled at.
Wherein, polyethers is that its viscosity is 40 ℃ of 20000～100000mm down by being polymerized of oxyethane and propylene oxide 1: 3 in molar ratio
2/ s; The weight-average molecular weight M=2000 of polyoxyethylene glycol～10000.
The effect of above-mentioned non-silicon type compound skimmer is the foam that reduces couplant, can adopt GXP-112-C, GXP-112-D etc.; The effect of spices auxiliary agent is to improve the couplant smell, can adopt rose compound, lotus essence.The dyestuff effect is an adjustment couplant color, can adopt neutral rose-red dyestuff etc.These auxiliary materials are used according to the general knowledge of concrete needs by this area.
Couplant for fault detection of the present invention is a non-mineral oil type couplant; And be water miscible; Therefore it can conveniently be removed by water; Composition attached to weld seam or overlay cladding surface evaporates in the subsequent heat treatment operation or voluntarily, perhaps can not produce harmful product, and couplant has anti-corrosion function in the flaw detection process and after the carrying out flaw detection, and it can protect the blue oxide film on overlay cladding surface can not change the brown iron rust into especially.The raw material sources of couplant for fault detection of the present invention is extensive, is common chemical materials, and product and production cost are lower, and can not produce harm to human body and environment.
The present invention also provides the method for preparing above-mentioned couplant for fault detection simultaneously, and this preparation method is simple, and preparation equipment is not had particular requirement.The preparation method of couplant for fault detection of the present invention; Comprise the steps: (1) preparation waterborne-type preservation; A. in the reaction unit that atmospheric condenser and TM are housed, adding lipid acid, epoxy compounds and purity by component is 99% nitrogenous compound, drips 98% vitriol oil; The control rate of addition, hierarchy of control temperature is within 50 ℃; B. be warming up to 185～195 ℃ after adding, insulation reaction 1.5～2.5 hours, the water that reaction generates is steamed simultaneously; C. cool off above-mentioned reactant, add excessive quicklime, distill, distillate is used anhydrous sodium sulfate drying; D. filter, filtrating adds an amount of activated carbon, refluxes then 30～50 minutes, and the cut of collecting 150～165 ℃ makes waterborne-type preservation; (2) in another reaction unit, add the waterborne-type preservation of producing through above-mentioned steps; Be warming up to the polyoxyethylene glycol that adds weight-average molecular weight M=2000～10000 after 90 ± 5 ℃ again; Fully stir; Reacted 25～45 minutes, (3) add polyoxyethylene glycol (molecular weight M=400～1000) and polyethers (20000～100000mm under 40 ℃
2/ s) viscosity of thing to be mixed reaches 40 ℃ of 50～150mm down
2/ s and acid number stopped to stir less than 0.01 o'clock; (4) naturally cooling is added the zero(ppm) water of surplus, makes water-soluble anti-corrosive type couplant for fault detection.In said step (4), when naturally cooling to below 80 ℃, also can add 0.01%～2% non-silicon type compound skimmer, dyestuff, spices auxiliary agent by weight percentage.
Below through the mode of specific embodiment the present invention is done further detailed description, be qualification but should not be construed as to subject area of the present invention, the technical scheme that all modifications of making based on the foregoing invention theme, replacement realize all belongs to protection scope of the present invention.Mm among the present invention
2/ s is meant the unit of viscosity; Acid number is represented the total amount of system middle acid substance, with the Pottasium Hydroxide milligram number of the required consumption of 1g resin, is unit with " mg/g " in being defined as.
Embodiment one preparation waterborne-type preservation
(1), in the reaction unit that atmospheric condenser and TM are housed, by 1 mole of component adding LAURIC ACID 99 MIN, 1.15 moles of nitrogenous compound pyridines; 0.2 mole of propylene oxide; Drip 98% vitriol oil, it is acid that the control rate of addition makes reaction system, and hierarchy of control temperature is within 50 ℃;
(2), be warming up to 185～195 ℃ after adding, insulation reaction 1.5～2.5 hours, the water that reaction generates is steamed simultaneously; C. cool off above-mentioned reactant, add excessive quicklime, distill, distillate is used anhydrous sodium sulfate drying;
(3), filter, filtrating adds an amount of activated carbon, refluxes then 30～50 minutes, collects 150～165 ℃ cut, makes waterborne-type preservation.
Repeat above-mentioned steps, the waterborne-type preservation of preparation aequum.
Embodiment two preparations couplant for fault detection of the present invention
(1) in the 2000ml three-necked bottle, add waterborne-type preservation 100 grams of embodiment one preparation, be warming up to the Liquid Macrogol gram that adds molecular weight 6000 after 90 ± 5 ℃ again, fully stir 25 minutes after, the acid number≤0.01mg/g of question response thing, viscosity reaches 1650mm
2After/s was above, adding polyoxyethylene glycol (molecular weight M=400) 500 grams and viscosity was 40 ℃ of following 25000mm
2Polyethers 250 grams of/s are heated to temperature and are controlled at 40 ℃～45 ℃, treat that the viscosity of product reaches 60～70mm
2Between/the s (under 40 ℃), acid number is less than 0.01 o'clock, stopped reaction;
(2) naturally cool to behind the stopped reaction below 80 ℃, add zero(ppm) water 340 grams of surplus after fully stirring, restir got final product in 3～5 minutes.So just obtain flaw detection of the present invention and use the anti-corrosive type couplant.
Embodiment three preparations couplant for fault detection of the present invention
(1) in the 3000ml three-necked bottle, adds waterborne-type preservation 200 grams that embodiment one prepares, be warming up to molecular weight 8000 polyoxyethylene glycol 100 grams that add again after 90 ± 5 ℃, fully stirred the acid number≤0.01mg/g of question response thing, viscosity>=1650mm 30 minutes
2Behind/the s, add polyoxyethylene glycol (molecular weight M=800) 790 grams, viscosity is 40 ℃ of following 45000mm
2The polyethers 350 of/s restrains, is heated to 45 ℃～50 ℃, treats that the viscosity of product reaches 60～70mm
2Between/the s (under 40 ℃), acid number is less than 0.01 o'clock, stopped reaction;
(2) naturally cool to behind the stopped reaction below 80 ℃; Geometric ratio adds auxiliary agent non-silicon type compound skimmer GXP-112-D, neutral rose-red dyestuff, lotus essence totally 10 grams (0.6%); Add zero(ppm) water 150 grams of surplus after fully stirring, restir got final product in 3～5 minutes.
Embodiment four preparations couplant for fault detection of the present invention
(1) in the 500ml three-necked bottle, adds waterborne-type preservation 90 grams that embodiment one prepares, be warming up to polyoxyethylene glycol 235 grams that add molecular weight 10000 after 90 ± 5 ℃ again, fully stirred the acid number≤0.01mg/g of question response thing, viscosity>=1650mm 40 minutes
2Behind/the s, add polyoxyethylene glycol (molecular weight M=1000) 50 grams, viscosity is 40 ℃ of following 65000mm
2/ s polyethers 10 grams are heated to temperature and are controlled at 40 ℃～45 ℃, treat that the viscosity of product reaches 60～70mm
2Between/the s (under 40 ℃), acid number is less than 0.01 o'clock, stopped reaction;
(2) naturally cool to behind the stopped reaction below 80 ℃, add auxiliary agent non-silicon type compound skimmer GXP-112-D, neutral rose-red dyestuff, lotus essence totally 1 gram, add zero(ppm) water 19 grams of surplus after fully stirring, restir got final product in 3～5 minutes.
Embodiment five preparations couplant for fault detection of the present invention
(1) in 10 liters of reaction kettles, adds 1.5 kilograms of the waterborne-type preservations of embodiment one preparation, be warming up to 1.8 kilograms of polyoxyethylene glycol that add molecular weight 6000 after 90 ± 5 ℃ again, fully stirred the acid number≤0.01mg/g of question response thing, viscosity>=1650mm 35 minutes
2Behind/the s, add polyoxyethylene glycol (molecular weight M=600) 2.5 kilograms, 40 ℃ of following 45000mm
2The polyethers of/s is heated to 45 ℃～50 ℃ for 0.2 kilogram, treats that the viscosity of product reaches 60～70mm
2Between/the s (under 40 ℃), acid number is less than 0.01 o'clock, stopped reaction;
(2) naturally cool to behind the stopped reaction below 80 ℃, add totally 0.02 kilogram of auxiliary agent non-silicon type compound skimmer GXP-112-C, neutral rose-red dyestuff, rose compound, add 1.48 kilograms of the zero(ppm) water of surplus after fully stirring, restir got final product in 3～5 minutes.
The Performance Detection test of Test Example one couplant of the present invention
The performance test results of above-mentioned each embodiment two to five obtained couplant is following:
1 coupling performance: UFSOFT join the PXUT-360 ultrasonic reflectoscope thickness be 200mm, stainless steel weld overlays thickness be carry out several kinds of couplants on the 70mm steel part comparison and detection consequently:
The couplant title; Machine oil glycerine industry paste various embodiments of the present invention are MV as a result
Wave height (Db) 10 20 15 36
Simultaneously, other acoustical behavior detected result MV of the couplant of various embodiments of the present invention preparation is: the velocity of sound (M/s): 1980; Specific acoustic resistance (* 10
6G/cm.s): 1.97, ultrasonic attenuation (dB/cm.M) :≤0.03
The rust resistance and corrosion resistance performance of 2 couplants of the present invention is as shown in table 1:
Table one coupling platform of the present invention agent performance test results
Therefore; From above-mentioned acoustical behavior, we can find out that couplant of the present invention compares with existing couplant at stainless steel surface and measured datas such as hyperacoustic coupling performance and rust resistance and corrosion resistance performance; Not only have good coupling performance, but also have antirust, anti-corrosive and technological advantage that other couplant does not possess fully.In addition; The raw materials for production cost of couplant for fault detection of the present invention is low, and toxicity is little, and the preparation method of couplant for fault detection of the present invention is simple simultaneously; Preparation equipment there is not particular requirement; The couplant for fault detection that obtains is safe and reliable to human body, for large-size chemical and nuclear power generating equipment weld seam and overlay cladding defect detecting test provide a kind of essential material of new excellent property, has good application prospects.
Claims (14)
1. couplant for fault detection, it is characterized in that: this couplant for fault detection contains by weight percentage:
Said waterborne-type preservation is prepared from through acid catalyzed reaction lipid acid, nitrogenous compound and three kinds of compositions of epoxy compounds; The mol ratio of used three kinds of compositions is: lipid acid 0.85～1.05, nitrogenous compound 0.95～1.25, epoxy compounds 0.15～0.3.
Said couplant for fault detection makes through following steps: (1) prepares water miscible sanitas: a. in the reaction unit that atmospheric condenser and TM are housed; Be 0.85～1.05: 0.95～1.25 in molar ratio: 0.15～0.3 adds lipid acid, nitrogenous compound and epoxy compounds respectively; Drip 98% vitriol oil; The control rate of addition is controlled within 50 ℃ with the guarantee system temperature; B. be warming up to 185～195 ℃ after adding, insulation reaction 1.5～2.5 hours, the water that reaction generates is steamed simultaneously; C. cool off above-mentioned reactant, add the quicklime of 2 times of amounts of sulfuric acid mole number, distill distillate and anhydrous sodium sulfate drying; D. filter, add the activated carbon of 1/8 volume in the filtrating, refluxed then 30～50 minutes, the cut of collecting 150～165 ℃ makes waterborne-type preservation;
(2) in another reaction unit, add the waterborne-type preservation of producing through above-mentioned steps, be warming up to the polyoxyethylene glycol that adds weight-average molecular weight M=2000～10000 after 50 ± 5 ℃, be heated to 120 ℃～140 ℃, fully stirred 25～45 minutes;
(3) add the polyoxyethylene glycol and the polyethers of molecular weight M=400～1000 again, the viscosity of treating product reach 40 ℃ down between 50～150mm2/s with acid number less than 0.01 o'clock, stopped reaction;
(4) naturally cooling is added the zero(ppm) water of surplus, makes water-soluble anti-corrosive type couplant for fault detection.
2. according to the said couplant for fault detection of claim 1, it is characterized in that: the carbochain of said lipid acid is C
6～C
18, at least a in caproic acid, sad, sebacic acid, LAURIC ACID 99 MIN, the oleic acid.
3. according to the said couplant for fault detection of claim 1, it is characterized in that: said nitrogenous compound is at least a in thanomin, diethylolamine, trolamine or the pyridine.
4. according to the said couplant for fault detection of claim 1, it is characterized in that: said epoxy compounds is at least a in oxyethane or the propylene oxide.
5. according to the said couplant for fault detection of claim 1, it is characterized in that: in the said catalytic reaction process, catalyzer is the sulfuric acid of concentration 98%, and its consumption shows acidity with the system of controlling to and is as the criterion.
6. according to the said couplant for fault detection of claim 1, it is characterized in that: said polyethers is to be polymerized in 1: 3 in molar ratio by oxyethane and propylene oxide, and its viscosity is 40 ℃ of 20000～100000mm down
2/ s.
7. prepare the method for the said couplant for fault detection of claim 1, comprise the steps:
(1) prepares water miscible sanitas: a. in the reaction unit that atmospheric condenser and TM are housed; Be 0.85～1.05: 0.95～1.25 in molar ratio: 0.15～0.3 adds lipid acid, nitrogenous compound and epoxy compounds respectively; Drip 98% vitriol oil; The control rate of addition is controlled within 50 ℃ with the guarantee system temperature; B. be warming up to 185～195 ℃ after adding, insulation reaction 1.5～2.5 hours, the water that reaction generates is steamed simultaneously; C. cool off above-mentioned reactant, add the quicklime of 2 times of amounts of sulfuric acid mole number, distill distillate and anhydrous sodium sulfate drying; D. filter, add the activated carbon of 1/8 volume in the filtrating, refluxed then 30～50 minutes, the cut of collecting 150～165 ℃ makes waterborne-type preservation;
(2) in another reaction unit, add the waterborne-type preservation of producing through above-mentioned steps, be warming up to the polyoxyethylene glycol that adds weight-average molecular weight M=2000～10000 after 50 ± 5 ℃, be heated to 120 ℃～140 ℃, fully stirred 25～45 minutes;
(3) add the polyoxyethylene glycol and the polyethers of molecular weight M=400～1000 again, treat that the viscosity of product reaches 40 ℃ of 50～150mm down
2Between/the s with acid number less than 0.01 o'clock, stopped reaction;
(4) naturally cooling is added the zero(ppm) water of surplus, makes water-soluble anti-corrosive type couplant for fault detection.
8. couplant for fault detection, it is characterized in that: this couplant for fault detection is composed of the following components by weight percentage:
Water is surplus; Wherein auxiliary agent is at least a in non-silicon type skimmer, dyestuff or the spices;
Said waterborne-type preservation is prepared from through acid catalyzed reaction lipid acid, nitrogenous compound and three kinds of compositions of epoxy compounds; The mol ratio of used three kinds of compositions is: lipid acid 0.85～1.05, nitrogenous compound 0.95～1.25, epoxy compounds 0.15～0.3;
Said couplant for fault detection makes through following steps: (1) prepares water miscible sanitas: a. in the reaction unit that atmospheric condenser and TM are housed; Be 0.85～1.05: 0.95～1.25 in molar ratio: 0.15～0.3 adds lipid acid, nitrogenous compound and epoxy compounds respectively; Drip 98% vitriol oil; The control rate of addition is controlled within 50 ℃ with the guarantee system temperature; B. be warming up to 185～195 ℃ after adding, insulation reaction 1.5～2.5 hours, the water that reaction generates is steamed simultaneously; C. cool off above-mentioned reactant, add the quicklime of 2 times of amounts of sulfuric acid mole number, distill distillate and anhydrous sodium sulfate drying; D. filter, add the activated carbon of 1/8 volume in the filtrating, refluxed then 30～50 minutes, the cut of collecting 150～165 ℃ makes waterborne-type preservation;
(2) in another reaction unit, add the waterborne-type preservation of producing through above-mentioned steps, be warming up to the polyoxyethylene glycol that adds weight-average molecular weight M=2000～10000 after 50 ± 5 ℃, be heated to 120 ℃～140 ℃, fully stirred 25～45 minutes;
(3) add the polyoxyethylene glycol and the polyethers of molecular weight M=400～1000 again, treat that the viscosity of product reaches 40 ℃ of 50～150mm down
2Between/the s with acid number less than 0.01 o'clock, stopped reaction;
(4) naturally cooling is added the zero(ppm) water of surplus, makes water-soluble anti-corrosive type couplant for fault detection;
In the said step (4), when naturally cooling to below 80 ℃, also add 0.01%～2% auxiliary agent by weight percentage, said auxiliary agent is at least a in non-silicon type skimmer, dyestuff or the spices.
9. said according to Claim 8 couplant for fault detection is characterized in that: the carbochain of said lipid acid is C
6～C
18, at least a in caproic acid, sad, sebacic acid, LAURIC ACID 99 MIN, the oleic acid.
10. said according to Claim 8 couplant for fault detection is characterized in that: said nitrogenous compound is at least a in thanomin, diethylolamine, trolamine or the pyridine.
11. said according to Claim 8 couplant for fault detection is characterized in that: said epoxy compounds is at least a in oxyethane or the propylene oxide.
12. said according to Claim 8 couplant for fault detection is characterized in that: in the said catalytic reaction process, catalyzer is the sulfuric acid of concentration 98%, and its consumption shows acidity with the system of controlling to and is as the criterion.
13. said according to Claim 8 couplant for fault detection is characterized in that: said polyethers is to be polymerized in 1: 3 in molar ratio by oxyethane and propylene oxide, and its viscosity is 40 ℃ of 20000～100000mm down
2/ s.
14. prepare the method for the said couplant for fault detection of claim 8, comprise the steps:
(1) prepares water miscible sanitas: a. in the reaction unit that atmospheric condenser and TM are housed; Be 0.85～1.05: 0.95～1.25 in molar ratio: 0.15～0.3 adds lipid acid, nitrogenous compound and epoxy compounds respectively; Drip 98% vitriol oil; The control rate of addition is controlled within 50 ℃ with the guarantee system temperature; B. be warming up to 185～195 ℃ after adding, insulation reaction 1.5～2.5 hours, the water that reaction generates is steamed simultaneously; C. cool off above-mentioned reactant, add the quicklime of 2 times of amounts of sulfuric acid mole number, distill distillate and anhydrous sodium sulfate drying; D. filter, add the activated carbon of 1/8 volume in the filtrating, refluxed then 30～50 minutes, the cut of collecting 150～165 ℃ makes waterborne-type preservation;
(2) in another reaction unit, add the waterborne-type preservation of producing through above-mentioned steps, be warming up to the polyoxyethylene glycol that adds weight-average molecular weight M=2000～10000 after 50 ± 5 ℃, be heated to 120 ℃～140 ℃, fully stirred 25～45 minutes;
(3) add the polyoxyethylene glycol and the polyethers of molecular weight M=400～1000 again, treat that the viscosity of product reaches 40 ℃ of 50～150mm down
2Between/the s with acid number less than 0.01 o'clock, stopped reaction;
(4) naturally cooling is added the zero(ppm) water of surplus, makes water-soluble anti-corrosive type couplant for fault detection;
In the said step (4), when naturally cooling to below 80 ℃, also add 0.01%～2% auxiliary agent by weight percentage, said auxiliary agent is at least a in non-silicon type skimmer, dyestuff or the spices.
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| CN2007102015162A CN101195703B (en) | 2006-09-19 | 2007-08-29 | Couplant for fault detection and method for producing the same |
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| CN200610021896.7 | 2006-09-19 | ||
| CN200610021896 | 2006-09-19 | ||
| CN2007102015162A CN101195703B (en) | 2006-09-19 | 2007-08-29 | Couplant for fault detection and method for producing the same |
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| CN101195703B true CN101195703B (en) | 2012-05-30 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101942165B (en) * | 2010-07-27 | 2012-01-11 | 上海诚友实业集团有限公司 | Nuclear grade ultrasonic inspection couplant and preparation method thereof |
| CN106959343A (en) * | 2017-03-20 | 2017-07-18 | 北京中鼎合信科技发展有限公司 | A kind of water base ultrasonic inspection couplant composition of environment-friendly high-efficiency and preparation method thereof |
| CN107367551B (en) * | 2017-07-04 | 2020-11-13 | 中国铁道科学研究院金属及化学研究所 | Coupling agent for ultrasonic flaw detection of steel rail welding seam |
| CN108132307B (en) * | 2017-10-26 | 2020-12-04 | 湖南金化科技集团有限公司 | Industrial coupling agent for steel rail flaw detection and preparation method thereof |
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Effective date of registration: 20180320 Address after: 618013 Deyang Pearl River West Road, Sichuan, No. 460 Patentee after: Double (Deyang) heavy equipment Co., Ltd. Address before: 618013 Deyang Pearl River West Road, Sichuan, No. 460 Patentee before: Erzhong Group (Deyang) Heavy Equipment Co., Ltd. |