CN102516913A - Environment-friendly flame-retardant fold adhesive and preparation method thereof - Google Patents
Environment-friendly flame-retardant fold adhesive and preparation method thereof Download PDFInfo
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- CN102516913A CN102516913A CN2011103950464A CN201110395046A CN102516913A CN 102516913 A CN102516913 A CN 102516913A CN 2011103950464 A CN2011103950464 A CN 2011103950464A CN 201110395046 A CN201110395046 A CN 201110395046A CN 102516913 A CN102516913 A CN 102516913A
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Abstract
The invention discloses an environment-friendly flame-retardant fold adhesive and a preparation method thereof, belongs to the technical field of single-component epoxy adhesives, and mainly solves the problem that the conventional epoxy resin fold adhesive cannot have good product mechanical properties and environment-friendliness and flame retardant properties simultaneously. The environment-friendly flame-retardant fold adhesive is mainly characterized by comprising 0 to 40 weight percent of epoxy resin, 5 to 50 weight percent of modified epoxy resin, 0 to 20 weight percent of diluent, 2 to 5 weight percent of curing agent, 0 to 5 weight percent of coupling agent, 1 to 20 weight percent of flame retardant, and 30 to 60 weight percent of filler. The method comprises the following steps of: (1) adding 0 to 40 weight percent of epoxy resin, 5 to 50 weight percent of modified epoxy resin, 0 to 20 weight percent of diluent, 2 to 5 weight percent of curing agent, 0 to 5 weight percent of coupling agent, 1 to 20 weight percent of flame retardant, and 30 to 60 weight percent of filler into a movable mixing machine, and uniformly stirring at the temperature of between 5 and 35 DEG C; and (2) vacuumizing in the movable mixing machine, stirring and defoaming, and discharging. The fold adhesive is environment-friendly and flame-retardant, is good in mechanical property, and is mainly used for adhesion of fold parts of an automobile.
Description
Technical field
The invention belongs to single-component epoxy glue technical field, be specifically related to a kind of environmental protection flame retardant automobile flanging tackiness agent and preparation method thereof, is to be applied in the technologic a kind of hot setting structure glue of weld car.This flanging glue environmental protection flame retardant, characteristics such as good mechanical performance.
Background technology
Epoxy resin flanging glue is good and bad because of its mechanical property, environmental protection, and cost is low, is the main flanging glue type of domestic and international automaker, like red flag, Buick, Audi, Santana, Dragon Lord Citroen zx etc.In recent years, domestic research to automobile flanging glue mainly concentrated on mechanical property, to the closely-related Study on flame retardance of vehicle safety performance but seldom.
At present, both at home and abroad to the environmental requirement special concern to the automotive industry auxiliary products of environmental issue growing interest, particularly European countries, a lot of full-sized car manufacturerss explicitly call for the material of forbidding to environment or human body harmful to its auxiliary products.Like french citroen company the materials used of automobile accessories product has been done clearly to limit, as: materials such as PBBs, PBDE, glycols, dimixo-octyl phthalate, cadmium, mercury, lead, sexavalent chrome.Wherein, PBBs, PBDE are as the use that is under an embargo of important fire retardant material; In addition; The flame retardant properties of common fire retardant is low, need just can reach flame retardant effect through heavy addition, but have a strong impact on product performance; As: the non-fire-retardant flanging glue of shearing resistance 30MPa, T stripping strength 145N/25mm is through the common fire retardant (as: white lake, Marinco H or its compsn) of interpolation 40%; Can reach fire-retardant requirement, but the product mechanical properties decrease is obvious, shearing resistance has only 15MPa, T stripping strength 30N/25mm.Can not improve product mechanical property and environmental protection flame retardant performance simultaneously, be a weak link of domestic flanging glue development.
In sum, develop a kind of environmental protection flame retardant, the automobile flanging glue of good mechanical performance is very necessary.
Summary of the invention
The present invention is directed to the above weak point of epoxy flanging glue and a kind of environmental protection flame retardant is provided, the automobile flanging glue of good mechanical performance.The present invention obviously improves flame retardant properties through adding a certain amount of special fire retardant.Not only flame retardant properties is good for automobile flanging glue through the present invention preparation, reach from fire burns time≤2s, and good mechanical performance, shearing resistance 29MPa, conservation rate 96.7%, T stripping strength 140N/25mm, conservation rate 96.6%.
The present invention also provides a kind of method for preparing above-mentioned automobile flanging glue.
The technical solution of environmental protection flame retardant automobile flanging glue of the present invention is: a kind of environmental protection flame retardant automobile flanging glue; The composition that it is characterized in that it comprises: 0% ~ 40%Wt epoxy resin, 5% ~ 50% Wt modified epoxy, 0% ~ 20%Wt thinner; 2% ~ 5%Wt solidifying agent; 0% ~ 5%Wt coupling agent, 1% ~ 20%Wt fire retardant, 30% ~ 60%Wt filler.
Said epoxy resin is glycidyl ether based epoxy resin, glycidyl ester based epoxy resin, Racemic glycidol amine epoxy resin, cycloaliphatic epoxy resin, epoxy olefines, imide ring epoxy resins, organosilicon epoxy resin or its compsn in the technical solution of the present invention.
Said modified epoxy is nano-rubber modified epoxy, carboxylic acrylonitrile butadiene rubber modified epoxy resin or its compsn in the technical solution of the present invention.Wherein, The nano-rubber modified epoxy is by the nano-rubber particle of epoxy resin and nucleocapsid structure or vulcanize nano-rubber entirely and form that (the nano-rubber modified epoxy sees Chinese invention patent application " a kind of automobile flanging glue and preparation method thereof ", application number: 200910273450.7) for details.The nuclear structure of the nano-rubber particle of nucleocapsid structure mainly contains polybutadiene rubber, styrene-butadiene rubber(SBR), polymethyl siloxane etc., and shell structure mainly contains methacrylic resin etc., has increased the intermiscibility of rubber particles and epoxy resin.Full sulfuration nano-rubber particle reduces from degree of crosslinking outside to inside gradually, and the center is reduced to minimum, and gradient crosslinked structure had not only kept the elasticity of rubber but also avoided the coalescence of particle, and the toughness of epoxy resin is greatly improved.Nano-rubber modified epoxy, carboxylic acrylonitrile butadiene rubber modified epoxy resin have improved the intensity and the toughness of cured article greatly; Especially nano-rubber modified epoxy; Very little in the time of toughness reinforcing to the influence of cured article storage modulus and second-order transition temperature; Can effectively improve the adhesiveproperties of pasta and non-pasta, like MX-125 (Japanese clock deep pool chemistry), MX-257 (Japanese clock deep pool chemistry), HH-0801 (West China, Shenzhen Hong Ji Science and Technology Ltd.).
Said thinner is reactive thinner, non-activated thinner or its compsn in the technical solution of the present invention, and wherein reactive thinner is meant and contains single epoxy group(ing) glycidyl ether, dioxygen base glycidyl ether or its compsn; Non-activated thinner is meant alkyl sulfonates, epoxy ester series, organic acid ester or its compsn.
Said solidifying agent is guanidine and verivate, urea and verivate thereof or its compsn in the technical solution of the present invention.
Said coupling agent is titanate coupling agent, silane coupling agent or its compsn in the technical solution of the present invention.
Said fire retardant is a red phosphorus combustion inhibitor in the technical solution of the present invention.
Said filler is MOX, carbonate, vitriol, silicon powder, silicate or its compsn in the technical solution of the present invention.
The preparation method of said a kind of environmental protection flame retardant automobile flanging glue in the technical solution of the present invention, it is characterized in that: this method may further comprise the steps:
1, with 0% ~ 40%Wt epoxy resin, 5% ~ 50% Wt modified epoxy, 0% ~ 20%Wt thinner; 2% ~ 5%Wt solidifying agent; 0% ~ 5%Wt coupling agent, 1% ~ 20%Wt fire retardant, 30% ~ 60%Wt filler add moving mixing in the machine; Stir down 10mim ~ 30min at 5 ℃～35 ℃, be uniformly dispersed to solid materials;
2, vacuumize stirring deaeration 30mim ~ 90min in the machine moving mixing, vacuum pressure is controlled at-0.09MPa, discharging.
Environmental protection flame retardant automobile flanging glue of the present invention is controlled limiting in the Industrial products with material is strict the environmental protection special concern, as: PBBs, PBDE, glycols, dimixo-octyl phthalate, cadmium, mercury, lead, sexavalent chrome.
Environmental protection flame retardant automobile flanging glue flame retardant properties of the present invention is good, selects the inorganic phosphorus flame retardant, have good flame retardation effect, Heat stability is good, non-volatile, do not produce corrosive gases, lasting, the low toxin of effect.
Environmental protection flame retardant automobile flanging glue good mechanical performance of the present invention uses the red phosphorus combustion inhibitor addition little, and little to the influence of product mechanical property, ordinary epoxy resin and modified epoxy are used, automobile flanging glue good mechanical performance.
The concrete performance index of automobile flanging glue of the present invention are seen table 1.
The present invention is mainly used in the bonding of flanging positions such as the car door, engine bonnet, luggage-boot lid of automobile.
Description of drawings
Fig. 1 is a test piece adhering method synoptic diagram of the present invention.
Fig. 2 is a T peel strength test test piece synoptic diagram of the present invention.
Fig. 3 is a T stripping strength test piece adhering method synoptic diagram of the present invention.
Fig. 4 is a T peel strength test method synoptic diagram of the present invention.
Fig. 5 is a T stripping strength load intensity diagram of the present invention.
Fig. 6 is a flame retardant properties test synoptic diagram of the present invention.
Embodiment
The following example and comparative example will be introduced the present invention more in detail, but the present invention is not limited to this.
Embodiment 1:
Proportioning
Epoxy resin (E-51) 20%Wt;
Nano-rubber modified epoxy (MX-125) 20%Wt;
Phenyl alkylsulf 5%Wt;
Dyhard RU 100 3%Wt;
Red phosphorus combustion inhibitor 3%Wt;
Titanate coupling agent (NDZ-101) 1%Wt;
Silicon powder 25%Wt;
Lime carbonate 23%Wt;
Preparation:
1, with 20%Wt epoxy resin (E-51), 20% Wt modified epoxy (MX-125), 5%Wt phenyl alkylsulf; The 3%Wt Dyhard RU 100,3%Wt red phosphorus combustion inhibitor, 1%Wt coupling agent NDZ-101; The 25%Wt silicon powder; 23%Wt lime carbonate adds moving mixing in the machine, stirs 20min down at 5 ℃～35 ℃, is uniformly dispersed to solid materials;
2, vacuumize stirring deaeration 60min in the machine moving mixing, vacuum pressure is controlled at-0.09MPa, discharging.
Performance test:
1, shearing resistance:
(1) test material: cold rolling steel disc, oil surface, 1.6mm is thick, and 25mm is wide, and 100mm is long.
(2) gluing: glue is scraped in the test piece with scraper.
(3) overlap joint test piece: tackiness agent scrapes after the test piece; By the glass microballon that in test piece, sprays shown in Figure 1, the medullary ray of two test pieces (a slice does not have gluing) of aliging is then fixed with two test pieces overlap joint and with clip at once; Before the curing, remove the glue that extrudes between test piece.
(4) test piece baking: behind the two test pieces overlap joint, under 180 ℃ * 30min condition, solidify, leave standstill cooling after, remove clip, the shape of test piece is as shown in Figure 1.
(5) normal temperature shearing resistance: at 23 ± 2 ℃, press GB/T 7124 test shearing resistances, draw speed is 50mm/min, record shearing resistance and destruction pattern.
2, T stripping strength
(1) test material: cold rolling steel disc, oil surface, 0.8mm is thick, and 25mm is wide, and 200mm is long, and shape is seen Fig. 2.
(2) gluing process: with the scraper applying glue to the test piece material.
(3) overlap joint test piece: tackiness agent scrapes after the test piece, at once by the glass microballon that in test piece, sprays shown in Figure 3, the medullary ray of two test pieces (a slice does not have gluing) of aliging then; Fix with two test pieces overlap joint and with clip; Before the curing, remove the glue that extrudes between test piece, like Fig. 3.
Test piece baking: behind the two test pieces overlap joint, under 180 ℃ * 30min condition, solidify, leave standstill cooling after, remove clip.
(4) T stripping strength: at 23 ± 2 ℃; Test the T stripping strength by Fig. 4, draw speed is 200mm/min, also remains 10mm with specified speed tensile test specimen up to gluing length; Through test; The trier load intensity diagram that draws is confirmed the average of test value from wavy load intensity diagram, record T stripping strength with destroy pattern.
Remarks: in beginning or test process, outlier possibly occur among the figure, this possibly should get rid of when calculating mean value, like Fig. 5 (unit: N/25mm) because defective or local gluing causing when unusual generation, mark out on figure unusually.
3, flame retardant properties:
(1) test material: cold-rolled steel sheet, 0.8mm is thick, and 75mm is wide, and 300mm is long.
(2) gluing process: to the test piece material, 0.8mm is thick with the scraper applying glue, and 75mm is wide, and 200mm is long, and shape is seen Fig. 6.
(3) flame retardant test: relative with the miter angle horizontal surface testing plate.Bunsen flame is adjusted to 38 millimeters.Maintain 18 millimeters (about 1/2 the length of flame) flames on test panel, effect continues 8 seconds.Remove flame, measure the testing plate duration of combustion.
Test result is seen table 1.
Embodiment 2:
Proportioning
Nano-rubber modified epoxy (MX-125) 45%Wt;
DINP 4%Wt;
5749 reactive thinner 10%Wt;
Dyhard RU 100 4%Wt;
Red phosphorus combustion inhibitor 1%Wt;
Silane coupling agent (KH-560) 1%Wt;
Talcum powder 15%Wt;
Lime carbonate 20%Wt;
Preparation technology and testing method are with embodiment 1, and test result is seen table 1.
Embodiment 3:
Proportioning
Epoxy resin (E-55) 35%Wt;
Nano-rubber modified epoxy (MX-257) 10%Wt;
5748 reactive thinner 5%Wt;
Dyhard RU 100 3%Wt;
Red phosphorus combustion inhibitor 10%Wt;
Titanate coupling agent (NDZ-401) 3%Wt;
Aluminum oxide 10%Wt;
Lime carbonate 24%Wt;
Preparation technology and testing method are with embodiment 1, and test result is seen table 1.
Embodiment 4:
Proportioning
Carboxyl LNBR modified epoxy 40%Wt;
5749 reactive thinner 5%Wt;
Phenyl alkylsulf 5%Wt;
Dyhard RU 100 3%Wt;
The chlorine wheat is swelled 1%Wt;
Red phosphorus combustion inhibitor 15%Wt;
Calcium sulfate 10%Wt;
Lime carbonate 21%Wt;
Preparation technology and testing method are with embodiment 1, and test result is seen table 1.
Embodiment 5:
Proportioning
Cycloaliphatic epoxy resin (the gloomy luxuriant CER-170 in Wuhan) 20%Wt;
Nano-rubber modified epoxy (MX-125) 30%Wt;
Dyhard RU 100 5%Wt;
Red phosphorus combustion inhibitor 3%Wt;
Titanate coupling agent (NDZ-102) 1%Wt;
Silicon powder 15%Wt;
Lime carbonate 26%Wt;
Preparation technology and testing method are with embodiment 1, and test result is seen table 1.
Embodiment 6:
Proportioning
4,4 ' MDA, four glycidyl amines (AG-80) 10%Wt;
Nano-rubber modified epoxy (MX-125) 20%Wt;
Epoxy soybean oil 5%Wt;
Dyhard RU 100 3%Wt;
Red phosphorus combustion inhibitor 3%Wt;
Titanate coupling agent (KH-401) 4%Wt;
Silicon powder 30%Wt;
Lime carbonate 25%Wt;
Preparation technology and testing method are with embodiment 1, and test result is seen table 1.
Comparative example 1:
Proportioning
Epoxy resin (E-51) 20%Wt;
Nano-rubber modified epoxy (MX-125) 20%Wt;
Phenyl alkylsulf 5%Wt;
Dyhard RU 100 3%Wt;
Titanate coupling agent (NDZ-101) 1%Wt;
Silicon powder 28%Wt;
Lime carbonate 23%Wt;
Preparation technology and testing method are with embodiment 1, and test result is seen table 1.
Comparative example 2:
Proportioning
Epoxy resin (E-51) 20%Wt;
Nano-rubber modified epoxy (MX-125) 20%Wt;
Phenyl alkylsulf 5%Wt;
Dyhard RU 100 3%Wt;
White lake 20%Wt;
Marinco H 20%Wt;
Titanate coupling agent (KH-401) 1%Wt;
Lime carbonate 11%Wt;
Preparation technology and testing method are with embodiment 1, and test result is seen table 1.
Claims (9)
1. an environmental protection flame retardant automobile flanging glue is characterized in that its composition comprises: 0% ~ 40%Wt epoxy resin, 5% ~ 50% Wt modified epoxy; 0% ~ 20%Wt thinner, 2% ~ 5%Wt solidifying agent, 0% ~ 5%Wt coupling agent; 1% ~ 20%Wt fire retardant, 30% ~ 60%Wt filler.
2. environmental protection flame retardant automobile flanging glue according to claim 1, it is characterized in that: said fire retardant is a red phosphorus combustion inhibitor.
3. environmental protection flame retardant automobile flanging glue according to claim 1 is characterized in that: said epoxy resin is glycidyl ether based epoxy resin, glycidyl ester based epoxy resin, Racemic glycidol amine epoxy resin, cycloaliphatic epoxy resin, epoxy olefines, imide ring epoxy resins, organosilicon epoxy resin or its compsn.
4. environmental protection flame retardant automobile flanging glue according to claim 1 is characterized in that: said modified epoxy is nano-rubber modified epoxy, carboxylic acrylonitrile butadiene rubber modified epoxy resin or its compsn.
5. environmental protection flame retardant automobile flanging glue according to claim 1; It is characterized in that: said thinner is reactive thinner, non-activated thinner or its compsn, and wherein reactive thinner is meant and contains single epoxy group(ing) glycidyl ether, dioxygen base glycidyl ether or its compsn; Non-activated thinner is meant alkyl sulfonates, epoxy ester series, organic acid ester or its compsn.
6. environmental protection flame retardant automobile flanging glue according to claim 1 is characterized in that: said solidifying agent is guanidine and verivate, urea and verivate thereof or its compsn.
7. environmental protection flame retardant automobile flanging glue according to claim 1 is characterized in that: said coupling agent is titanate coupling agent, silane coupling agent or its compsn.
8. environmental protection flame retardant automobile flanging glue according to claim 1 is characterized in that: said filler is MOX, carbonate, vitriol, silicon powder, silicate or its compsn.
9. method for preparing the described environmental protection flame retardant automobile of claim 1 flanging glue is characterized in that may further comprise the steps:
(1) with 0% ~ 40%Wt epoxy resin, 5% ~ 50% Wt modified epoxy, 0% ~ 20%Wt thinner; 2% ~ 5%Wt solidifying agent; 0% ~ 5%Wt coupling agent, 1% ~ 20%Wt fire retardant, 30% ~ 60%Wt filler add moving mixing in the machine; Stir down 10mim ~ 30min at 5 ℃～35 ℃, be uniformly dispersed to solid materials;
(2) vacuumize stirring deaeration 30mim ~ 90min in the machine moving mixing, vacuum pressure is controlled at-0.09MPa, discharging.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965063A (en) * | 2012-11-25 | 2013-03-13 | 广东普赛特电子科技股份有限公司 | Nanometer modified red gum and preparation method thereof |
| CN107236515A (en) * | 2017-06-17 | 2017-10-10 | 常州新区金利宝塑料制品有限公司 | A kind of preparation method of automobile folding adhesive |
| CN107345124A (en) * | 2017-08-09 | 2017-11-14 | 盐城市宝光车用材料有限公司 | A kind of high intensity folding adhesive |
| CN116004160A (en) * | 2022-12-29 | 2023-04-25 | 保光(天津)汽车零部件有限公司 | Automobile hemming adhesive, preparation method and application |
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| CN1621478A (en) * | 2003-11-28 | 2005-06-01 | 三友（天津）高分子技术有限公司 | Flexible adhesive compositions |
| CN102115654A (en) * | 2009-12-30 | 2011-07-06 | 湖北回天胶业股份有限公司 | Automobile hemming adhesive and preparation method thereof |
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| CN1621478A (en) * | 2003-11-28 | 2005-06-01 | 三友（天津）高分子技术有限公司 | Flexible adhesive compositions |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965063A (en) * | 2012-11-25 | 2013-03-13 | 广东普赛特电子科技股份有限公司 | Nanometer modified red gum and preparation method thereof |
| CN107236515A (en) * | 2017-06-17 | 2017-10-10 | 常州新区金利宝塑料制品有限公司 | A kind of preparation method of automobile folding adhesive |
| CN107345124A (en) * | 2017-08-09 | 2017-11-14 | 盐城市宝光车用材料有限公司 | A kind of high intensity folding adhesive |
| CN116004160A (en) * | 2022-12-29 | 2023-04-25 | 保光(天津)汽车零部件有限公司 | Automobile hemming adhesive, preparation method and application |
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Application publication date: 20120627 |