CN102329593B - High-strength structural adhesive - Google Patents
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- CN102329593B CN102329593B CN 201110311988 CN201110311988A CN102329593B CN 102329593 B CN102329593 B CN 102329593B CN 201110311988 CN201110311988 CN 201110311988 CN 201110311988 A CN201110311988 A CN 201110311988A CN 102329593 B CN102329593 B CN 102329593B
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Abstract
The invention provides a high-strength structural adhesive and a preparation method thereof. After a repairing agent is cured, an adhesive layer is milk yellow and has the binding strength of 56MPa, the use temperature of (-60)-180 DEG C, as well as good oil resistance, water resistance, weak-acid resistance, base resistance and impact resistance; and the structural adhesive is mainly applied in adhesive bonding and adhesive coating of important structural stress parts, such as adhesive bonding and repair of shafts, box cracks and fractured component structures.
Description
Technical field
The present invention relates to a kind of high strength structural adhesion, especially a kind of high-strength structure healant of epoxide modified normal temperature cured type excellent combination property.
Background technology
Surface Engineering is paid much attention to day by day as the important means of maintenance.As Surface Engineering subject important component part n9 sufacing, the surface recovery technique comprises plating, Brush Plating, thermospray, bonding snearing etc., these restorative procedures replenish mutually, become the means emergency schedule of maintenance of equipment necessity, repair scrapped parts, old part is come back to life, and for enterprise retrieves the tremendous economic loss, maintenance of equipment has become the organic component of productivity.
The surface cohering technology is as one of Modern Surface Technology, in recent years, brought into play significant role and obtained good social benefit and huge economic benefit in the maintenance of equipment field.
The surface cohering technology is compared with built-up welding, thermospray, Brush Plating, its simple process, do not need Special Equipment, need not to consume heat energy and electric energy, only need the surface to be repaired that it is good that the healant for preparing is coated on cleaning is got final product, after solidifying as hard as metal, can carry out various mechanical workouts, satisfy the maintenance needs such as part wetted surface, anti-corrosion, resizing, defective are filled up, sealing and plugging.General ambient temperature curable, to part without heat affected zone and thermal distortion, but and site work, reduce stop time.Its time and labour saving, save energy and substantial contribution are a kind of quick and inexpensive repairing techniques, are the effective means of maintenance of equipment, will develop into one of important Modern Surface Technology.
metal repairing agent is the gordian technique of surface cohering and splicing in maintenance of equipment, it is by high molecular polymer and metal-powder, ceramic powder and fibrous pair of component (or many components) clay shape matrix material, being widely used in the part wetted surface damages, corrosion-resistant reparation is with pre-supercoat and be used for repairing the various defectives of part (as crackle, scratch, dimension overproof, blow hole, sand holes) and sealing and plugging etc., its simple process is easily gone, only need two components are mixed in proportion, be coated on through rust cleaning, the surface of oil removing, after solidifying, finishing gets final product, a kind of saving of labor, save time, economical, durable, flexibly, convenient, desirable Novel patching material, it is one of matrix material at present with fastest developing speed.
This patching material abroad just begins one's study from the fifties end, U.S. Belzona high polymer alloy healant for example, Germany Diamant product is also world-famous, can be used to repair various materials, can be used for repairing metal, rubber, pottery etc., can select the healant of the different trades mark according to conditions such as different use temperatures, pressure, media.The MEcATeC product of Switzerland Castolin company also has tens kinds, is widely used in the maintenance of equipment of the multiple industries such as casting, cement, sugaring, railway, electronics.In addition, fill up agent, wetted surface glue although more domestic units develop some metals, performance can't satisfy the service requirements of maintenance of equipment.The patching material of above-mentioned external development, although performance is higher than home products, China's the eighties was just once used German Diamant product to the tank track hanging rubber plate, but intensity, heat resistance still are difficult to reach the requirement of the equipment of repairing the performance requriements harshnesses such as war industry equipment or intensity, and the price of import healant and costliness thereof, consume a large amount of foreign exchanges, cause enterprise to consume a huge sum of money aspect maintenance of equipment.
The series high strength structure glue of the present invention's development is the high-strength structure healant of epoxide modified normal temperature cured type excellent combination property, minute A, B two components; The A component is the light grey clay shape of main glue, and the B component is solidifying agent oyster white clay shape, and the cured glue layer is canescence; After solidifying, bonding strength is high, and heatproof, oil resistant, water-fast, ageing-resistant are applicable to the structural adhesive bonding of various device part breaking.
Summary of the invention
The composition of healant can be divided into sizing, solidifying agent, toughner, particular fillers, thinner, coupling agent, anti-aging agent, thixotropic agent, defoamer, promotor etc.Sizing is selected epoxy resin, resol, unsaturated polyester, urethane, silicone resin etc., and filler can be divided into metal-powder (as iron powder, aluminium powder, copper powder, lead powder etc.), ceramic powder (WC, SiC, A1
2O
3, BC, Cr
2O
3, SiO
2, quartz sand etc.) and graphite, MoS
2, the antifriction materials such as polytetrafluoroethylene.Two two component healants, during coating, two components are mixed use by a certain percentage, generally are comprised of sizing, solidifying agent and filler (abbreviation particular fillers) and subsidiary material with certain characteristic (wetted surface, against corrosion, insulation, conduction etc.).
1, sizing
Or the title base-material, as thermosetting resin, synthetic rubber etc.Thermosetting resin such as epoxy, phenolic aldehyde, urethane, unsaturated polyester, acrylic acid ester etc. have the three-dimensional crosslinking structure, and are heat-resisting, water-fast, resistance to medium is good, use more in healant.
The effect of sizing is the various materials in healant to be contained and stick to securely matrix surface to form coating, therefore, and for the sizing of adhesive coating layer should have following performance:
(1) coated matrix and filler there is higher bonding strength.
(2) cured article should have higher physical strength and good heatproof, oil resistant, chemically-resistant and ageing resistance, and its Young's modulus and stability want high.
(3) the cured article shrinking percentage is little.
2, solidifying agent
The effect of solidifying agent is and sizing generation chemical reaction, forms netted space polymer, and the filler envelope in the body of dictyosome, is formed the crosslinked combination of three-dimensional.
Requirement with solidifying agent is generally to healant:
(1) cured article hardness is high, good toughness, and wetted surface is good, and solidity to corrosion, medium-resistance are good etc.
(2) preferably can self-vulcanizing, set time is short.
Healant of the present invention is generally amine curing agent with solidifying agent, adopts aminated compounds as solidifying agent, makes healant that higher degree of cure and outstanding resistance toheat be arranged.
3, particular fillers
Particular fillers plays very important effect in healant, as antiwear and antifriction, anti-corrosion, insulation, conduction etc.Therefore the selection of particular fillers is most important to the performance of coating, needs and the chemical terms consideration from maintenance, filler is required be:
(1) filler should be neutral or weakly alkaline, does not contain in conjunction with water, and is good with the sizing affinity, to liquid without adsorptivity or adsorptivity seldom arranged.
(2) filler absorption impurity enough thermotolerances and certain purity will be arranged, if can cause the resin degraded.
(3) require particle or grain density little, scattered, sedimentation is little in resin.
The healant filler comprises powder or the fiber with a certain size; as metal-powder, oxide compound, carbide, the nitride even hard particles such as diamond, boride or fiber, graphite, molybdenumdisulphide, polytetrafluoroethylene etc., the wear-resistant filler of hard optional according to different coatings.
4, subsidiary material
Subsidiary material comprise toughner, plasticity, thinner, curing catalyst, coupling agent, defoamer, anti-aging agent etc., its effect be improve coating performance such as toughness, resistance to deterioration etc. and reduce glue viscosity, improve coating quality etc.
According to above-mentioned four kinds of component roles, according to different working conditionss and performance requriements, through testing preferred suitable material and proportioning, the healant of preparation various requirement.
In addition, the present invention also provides the production method of above-mentioned high strength structural adhesion.
The invention provides a kind of high strength structural adhesion, mixed by A component and B component, wherein the A component is epoxy resin E44, epoxy resin E51, aluminium sesquioxide, Stainless Steel Powder, titanium dioxide, 100 order white carbon blacks and 400 order white carbon blacks; The B component is KH550 silane coupling agent, DMP-30(2,4,6-three (dimethylamino methyl) phenol), aluminium sesquioxide and white carbon black; The weight proportion of A component and B component is 3:1 ~ 5:1, and optimum ratio is 4:1.
The formula that adopts in concrete production process is as follows: the A component is epoxy resin E44 9750g, epoxy resin E51 600g, aluminium sesquioxide 1885g, Stainless Steel Powder 303g, titanium dioxide 156g, 100 order white carbon black 90g and 400 order white carbon black 150g; The B component is KH550 silane coupling agent 45g, DMP-30(2,4,6-three (dimethylamino methyl) phenol) 690g, aluminium sesquioxide 146g and white carbon black 1200g; The use of healant is the ratio of 3:1 ~ 5:1 with above-mentioned A, B component by weight ratio, and the ratio of preferred 4:1 takes, and mixes.
High strength structural adhesion by the said ratio preparation, the cured glue layer is milk yellow, bonding strength reaches 56MPa, use temperature is-60～180 ℃, oil resistant, water-fast, weak acid resistant, alkali, impact resistance are good, be mainly used in splicing and the snearing of important feature force part, as axle class, casing crackle and broken pieces structural adhesive bonding and reparation.
The preparation method of high strength structural adhesion of the present invention comprises the steps:
1. use area of computer aided coating formula optimization design, obtain the formula of above-mentioned healant;
At first starting material have been carried out preferably, by a large amount of simultaneous tests, and then the factor such as filling kind, filling adding amount, filler granularity, solidifying agent, toughner kind and the add-on that affect coating wetted surface, hardness, intensity have been carried out single factor experiment, determined the optimum range of each composition, with the design of computer assistant coating formulation optimization, obtain optimum formula at last.
The process that the area of computer aided coating is optimized is as follows: the design of Variable Factors level---formula test------formula optimization---optimization formula of setting up mathematical model.
By result as can be known, the high strength structural adhesion coating formula performance of computer aided optimum obviously improves, and compares with the formula of general extremum method optimization, approximately improves 20%.
2. starting material are anticipated;
1) starting material in bulk and that make moist are dried under 100 ℃;
2) starting material of thickness added heat gain mobility, but temperature can not surpass 60 ℃, with anti-metamorphic;
3) to coarse grained pulvis starting material, grind and sieve and get fine particle materials;
3.A, the preparation of B component
Take A component starting material by formula, epoxy resin E51, epoxy resin E44 are placed in double-planet dynamic mixing still, be heated to 90 ℃, stir 30min, add aluminium sesquioxide, Stainless Steel Powder, titanium dioxide, 100 orders and 400 order white carbon blacks, then high-speed stirring 30min is cooled to 40 ℃ to mixing, vacuumize and stirring at low speed 20min, obtain the A component standby;
Take B component starting material by formula, KH550 silane coupling agent and DMP-30 are placed in double-planet dynamic mixing still, and mix and blend 30min adds aluminium sesquioxide and white carbon black to continue to stir 30min to mixing, then vacuumize and stirring at low speed 20min, obtain the B component standby;
4. the preparation of healant
Press A, B two component weight ratio A:B=3:1 ~ 5:1, the ratio weighing of preferred 4:1 is taken out, namely use after stirring, the glue for preparing is when 20 ℃ of left and right of room temperature, be preferably in 30 ~ 40min and be finished, in order to avoid viscosity increase affect tackiness agent with by infiltration and the bonding snearing effect of sticking part, how much join the glue amount depending on correction of the defect big or small, matching while using.
Using method:
1, position to be repaired purifies with the decontamination of acetone (analytical pure) degreasing degreasing;
2, the available file in surface to be repaired, sand paper (cloth), hand operated grinding wheel, the rotary file roughening treatment, roughness is advisable, car goes out cutter flower (60 ° of sharp knives but glued joint also to axle or pore structure, ap=0.4, f=0.755), the most handy needle file double thread suitably alligatoring again after car goes out.
3, structural adhesive bonding or the groove for axle, cover connects, and tolerance clearance is monolateral is advisable at 0.05 ~ 0.15m, is generally 0.1mm, avoids glue-line too thick too thin.
4, be coated with adhesive curing, avoid constructing under greater than 90% environment lower than 5 ℃ of following humidity in temperature, generally can spontaneous curing more than 15 ℃, if the heating cure Joint strength can greatly improve (be coated with when being heating and curing the gummed disturb heat after 1 hour 30 ℃ 1 hour, heat up again 50 ~ 60 ℃ 2 hours, slow cooling then).Precaution
Storing the quality guaranteed period is 2 years.
Useful technique effect of the present invention is:
1, high strength structural adhesion ultimate compression strength of the present invention is high, surpasses 82MPa; 2,56MPa coated matrix had higher bonding strength, more than can be reached.
Description of drawings
Fig. 1 is tension specimen;
Fig. 2 is for shearing sample;
Fig. 3 is compressive sample;
Fig. 4 is the wearing test sample.
Embodiment
Below in conjunction with embodiment 1-3, the present invention is further described in detail, but the present invention never is confined to these embodiment.
Embodiment 1-3
The A component is epoxy resin E44 9750g, epoxy resin E51 600g, aluminium sesquioxide 1885g, Stainless Steel Powder 303g, titanium dioxide 156g, 100 order white carbon black 90g and 400 order white carbon black 150g; The B component is KH550 silane coupling agent 45g, DMP-30(2,4,6-three (dimethylamino methyl) phenol) 690g, aluminium sesquioxide 146g and white carbon black 1200g; The use of healant for the ratio of 3:1 ~ 5:1 takes, mixes above-mentioned A, B component by weight ratio.The concrete proportioning of each embodiment is as shown in table 1.
Table 1
| |
1 | 2 | 3 |
| The trade mark | TCY800 | TCY801 | TCY802 |
| A, B ratio | 3:1 | 4:1 | 5:1 |
Tensile strength, tensile shear strength, compressive strength, hardness, wetted surface, 7 performance index of erosion resistance and temperature tolerance are tested by the Ministry of Chemical Industry and national standard, and testing method and test result are as follows:
3.1 tensile strength
(1) testing method:
1, sample (specimen shape, size are as shown in Figure 1)
Attention: the splicing face of sample should be the plane, and vertical with the main shaft of sample; Adhesively bonded joint should use the tackiness agent of capacity, and makes the glue of slightly having a surplus around joint, avoids occurring starved joint, and excessive glue needn't be removed usually.
2, testing installation:
Puller system should make the sample failure load at 10%～90% of pulling force full range, and the measuring error of puller system is not more than 1%, and puller system should be able to constant speed ground increase load.
3, test conditions:
When there is no particular requirement, the test conditions of recommending by GB2918 carries out, and namely temperature is 23 ± 2 ℃, relative humidity (50 ± 5) %.
4, test-results:
(1) tensile strength is calculated by formula (1):
Maximum load (N) when P one sample destroys;
A one bond area (mm2).
(2) unless regulation is separately arranged in the adhesive products standard, tensile strength values is in the arithmetical av of five efficiency test results.
(2) test result
Tensile strength test the results are shown in Table 2.
Table 2 tensile strength test result
3.2 tensile shear strength
Testing method:
1, sample
On specimen shape to the greatest extent cun as shown in Figure 2.
2, testing installation
(1) failing load that the trier that uses should make sample the full scale load 15%～85% between, the power value indication error of trier should be greater than 1%, trier should guarantee that the translational speed of specimen holder keeps stablizing among 5 ± 1mm/1min;
(2) glueing joint the tinsel surface of use should be smooth, the bending that do not have, lifts up song, the distortion such as crooked.Tinsel should be without burr, and the edge keeps the right angle;
(3) the preparation sample all should use fixture, to guarantee that sample correctly overlaps and accurately to locate.
3, test conditions
Unless otherwise prescribed, the storage period of sample and testing circumstance should meet the following requirements:
(1) shortest time to test after sample prepares is 16h, and maximum duration is 1 month:
(2) test should be carried out in temperature is the environment of 23 ± 2 ℃.Arbitration test or should be that 234 ± 2 ℃, relative humidity are to carry out in 45%～55% environment in temperature to the tackiness agent of temperature, humidity sensitive;
(3) to the test of temperature requirement is only arranged, before test, sample storage period under test temperature should not be less than half an hour; To the test of temperature, humidity requirement is arranged, before test, the storage period of sample under testing circumstance generally should not be less than 16h.
4, test-results
(1) tensile shear strength calculates by formula (2):
In formula
--tensile shear strength (MPa);
Maximum load (N) when P--destroys;
B--sample bonding plane width (mm);
L--sample bonding plane length (mm).
(2) test-results represents with arithmetical av, maximum, the Schwellenwert of shearing resistance, gets four position effective digitals.
(2) test result
The tensile shear strength test-results sees Table 3.
Table 3 tensile shear strength test-results
3.3 ultimate compression strength
(1) testing method
1, sample
(1) glue Chinese catalpa shape, size are as shown in the figure
(2) upper and lower end face of glue post should be the plane, and vertical with the main shaft of glue post.
2, testing installation
Trier should make the sample failure load at 10%～90% of full range, and the measuring error of trier is not more than 1%.
3, test conditions
The pressure head of testing machine translational speed is ± 0.2mm/min.
4, test-results
(1) ultimate compression strength is calculated by formula (3);
B=P／A
B one ultimate compression strength (MPa) in formula;
Maximum load (N) when P one destroys;
A one glue post cross-sectional area (mm
2).
(2) test result
Table 4 compressive strength test result
3.4 hardness
(1) testing method:
1, sample
(1) glue-line is answered even thickness, smooth surface, smooth, without bubble, have no mechanical damage and impurity etc.;
(2) bondline thickness should be not less than 3 millimeters;
(3) sample size should guarantee that each measurement point and sample Edge Distance are not less than 12 millimeters, and the distance between each measurement point is not less than 6 millimeters;
(4) every group of sample measurement counted and is no less than 5, can carry out on one or several sample.
2, testing installation
(1) this test equipment used is the xHS.D Shore durometer.
(2) hardness permission maximum deviation is ± 1 Shore durometer number.
3, test conditions
During (1) without particular requirement, before test, sample should be placed in testing circumstance 1 hour at least.
(2) pressing and reading immediately after sample contacts 15 seconds fully, if regulation is wanted instantaneous reading, contact reading in rear 1 second at pressing and sample fully.
4, test-results
(1) reading that obtains on the reading scale is the Shore durometer number of measuring.
(2) every group of sample measurement counted and is no less than 5, can carry out on one or several sample, and test-results is with the arithmetical mean value representation of one group of sample.
(2) test result
Hardness test the results are shown in Table 5.
Table 5. the hardness test result
3.5 wetted surface
(1) testing method
1, sample
(1) specimen shape, size are as shown in Figure 4;
(2) matrix of samples is 45 steel, and coating is combined with matrix firmly, the coatingsurface zero defect.
2, testing installation
(1) this test equipment used is SKODA-SAVIN friction wear testing machine;
(2) emery wheel is 40 Wimet, surface roughness Ra 0.03;
(3) emery wheel rotating speed: n=675r/rain.
3, test conditions
(1) before the test, specimen surface polishes;
(2) preload: p=5Kg;
(3) total revolution: N=3000r;
(4) emery wheel be coated with interlayer spray 50%K
2CrO
7The aqueous solution.
4, test-results
(1) measure the polishing scratch width B with eyepiece, tabling look-up draws corresponding wear volume, calculates its wetted surface;
(2) test-results is to be no less than the arithmetical mean value representation of three test blocks.
(2) test result
Wearing test the results are shown in Table 6
Table 6. wearing test result
3.6 erosion resistance
(1) test method
1, sample
Cast out 20 * 24 sample with plastics tubing
2, corrosive fluid
Preparation 20%, 30% hydrochloric acid soln, 20%, 30%, 50%, 70% sulphuric acid soln, 20%, 30 %, 50%, 70% sodium hydroxide solution, 10%NaCl solution and measure toluene.
3, test conditions
(soil) test is at room temperature carried out;
(2) regularly observe, record observations after surrounding.
(2) test-results
Anti-corrosion test the results are shown in Table 7.
Table 7. anti-corrosion test result
In 2 tables "/" be that no this item is tested
3.7 temperature tolerance
(1) testing method
1, sample
Tackiness agent evenly is coated in 45 steel matrix surperficial, bondline thickness 2mm.
2, test conditions
The sample that snearing is good is put into baking oven, progressively heat to the desired temperature of test, after the insulation certain hour, observe the glue-line changing conditions.
(2) test result
The temperature tolerance test-results sees Table 8.
Table 8 heatproof test-results
Claims (3)
1. high strength structural adhesion, mixed by A component and B component, it is characterized in that, wherein the A component is epoxy resin E44 9750g, epoxy resin E51 600g, aluminium sesquioxide 1885g, Stainless Steel Powder 303g, titanium dioxide 156g, 100 order white carbon black 90g and 400 order white carbon black 150g; The B component is KH550 silane coupling agent 45g, DMP-30(2,4,6-three (dimethylamino methyl) phenol) 690g, aluminium sesquioxide 146g and white carbon black 1200g; The weight proportion of A component and B component is 3:1 ~ 5:1.
2. high strength structural adhesion according to claim 1, is characterized in that, the weight proportion of A component and B component is preferably 4:1.
3. the preparation method of according to claim 1-2 described high strength structural adhesions of any one, comprise the steps:
1) use area of computer aided coating formula optimization design, obtain the formula of above-mentioned healant;
2) starting material are anticipated; Wherein, starting material are anticipated comprise: 1. starting material in bulk and that make moist are dried under 100 ℃; 2. the starting material of thickness added heat gain mobility, but temperature can not surpass 60 ℃, with anti-metamorphic; 3. to coarse grained pulvis starting material, grind and sieve and get fine particle materials;
3) preparation of A, B component
Take A component starting material by formula, epoxy resin E51, epoxy resin E44 are placed in double-planet dynamic mixing still, be heated to 90 ℃, stir 30min, add aluminium sesquioxide, Stainless Steel Powder, titanium dioxide, 100 orders and 400 order white carbon blacks, then high-speed stirring 30min is cooled to 40 ℃ to mixing, vacuumize and stirring at low speed 20min, obtain the A component standby;
Take B component starting material by formula, KH550 silane coupling agent and DMP-30 are placed in double-planet dynamic mixing still, and mix and blend 30min adds aluminium sesquioxide and white carbon black to continue to stir 30min to mixing, then vacuumize and stirring at low speed 20min, obtain the B component standby;
4) preparation of healant
Ratio weighing in A, B two component weight ratios is taken out, and namely uses after stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110311988 CN102329593B (en) | 2011-10-15 | 2011-10-15 | High-strength structural adhesive |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110311988 CN102329593B (en) | 2011-10-15 | 2011-10-15 | High-strength structural adhesive |
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| CN102329593B true CN102329593B (en) | 2013-05-08 |
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|---|---|---|---|
| CN 201110311988 Expired - Fee Related CN102329593B (en) | 2011-10-15 | 2011-10-15 | High-strength structural adhesive |
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| CN102879268B (en) * | 2012-05-31 | 2014-07-16 | 同济大学 | Method for detecting sheet cementing piece strength based on curing degree |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4665111A (en) * | 1984-10-12 | 1987-05-12 | Siemens Aktiengesellschaft | Casting compound for electrical and electronic components and modules |
| CN101619201A (en) * | 2009-07-16 | 2010-01-06 | 青岛红树林投资有限公司 | Underwater epoxy adhesive and preparation method thereof |
| CN101851481A (en) * | 2010-05-22 | 2010-10-06 | 东方电气集团东方汽轮机有限公司 | Epoxy resin adhesive for manufacturing blades of wind driven generator and preparation method thereof |
-
2011
- 2011-10-15 CN CN 201110311988 patent/CN102329593B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4665111A (en) * | 1984-10-12 | 1987-05-12 | Siemens Aktiengesellschaft | Casting compound for electrical and electronic components and modules |
| CN101619201A (en) * | 2009-07-16 | 2010-01-06 | 青岛红树林投资有限公司 | Underwater epoxy adhesive and preparation method thereof |
| CN101851481A (en) * | 2010-05-22 | 2010-10-06 | 东方电气集团东方汽轮机有限公司 | Epoxy resin adhesive for manufacturing blades of wind driven generator and preparation method thereof |
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