CN102746796A - Bi-component acrylic ester structure adhesive and preparation method thereof - Google Patents

Bi-component acrylic ester structure adhesive and preparation method thereof Download PDF

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Publication number
CN102746796A
CN102746796A CN2012101610388A CN201210161038A CN102746796A CN 102746796 A CN102746796 A CN 102746796A CN 2012101610388 A CN2012101610388 A CN 2012101610388A CN 201210161038 A CN201210161038 A CN 201210161038A CN 102746796 A CN102746796 A CN 102746796A
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stirred
monomer
polyurethane prepolymer
promotor
added
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史富永
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YANTAI SEAYU ELECTRONIC CO., LTD.
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YANTAI SEAYU ELECTRONIC CO Ltd
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Abstract

The invention discloses a bi-component acrylic ester structure adhesive and a preparation method thereof. According to the invention, a monomer, an elastomer, toughening resin, a polyurethane prepolymer, and methacrylic acid are added into a reaction vessel, such that a uniform liquid can be obtained in the reaction vessel; gamma-methacryloyloxy trimethoxy silane, N,N-dimethyl-p-toluidine, and a peroxide are added to the liquid; the mixture is stirred, such that a main agent is obtained. When a promoting agent comprises two components, biphenyl-A epoxy resin is added into a reaction vessel; the mixture is stirred under normal temperature; vanadium salt is added, and stirring is continued, such that the promoting agent is prepared. A monomer, toughening resin, an elastomer, and a polyurethane prepolymer are added into a reaction vessel, and are stirred, such that a uniform liquid is obtained; the promoting agent and an inorganic filling material are added to the liquid, and the mixture is stirred, such that a curing agent is obtained. The adhesive is advantaged in fast heating positioning. When the adhesive is mixed, a storage life of the adhesive under normal temperature is long, adhesive application is convenient, and a shear strength is high.

Description

A kind of two-component acrylicester structural adhesive and preparation method thereof
Technical field
The invention belongs to the acrylic ester structural adhesive technical field, be specifically related to a kind of two-component acrylicester structural adhesive and preparation method thereof
Background technology
Because fast type acrylate adhesive admittedly has distinguishing features such as room temperature fast-curing, intensity height, H.T. and shock resistance; Therefore the construction bonds that is widely used in Aeronautics and Astronautics, automobile, machinery, electronics, electrical equipment or the like industry, equipped, big part assembling of smallclothes and leak stopping reparation etc.High-endly also obtained good application aspect scientific and technological at some.
The curing mode of two-component acrylicester sizing agent can make glue fixed bit just usually earlier at a certain temperature at present, heats 20-30 minute to reach completely solidified in 24 hours or 60-80 ℃ in room temperature afterwards.And in the first fixed bit of glue, need apply certain pressure to corresponding bonded part, in case the glue no-fix causes the bonded part cracking.Therefore, short more progress that more can faster production of the time of the first fixed bit of two-component acrylicester sizing agent, but set time is too short; Can make the running time too of short duration again; Generation is untimely because of operating, and the sizing agent solidified situation that do not put in place promptly causes unnecessary waste.
Summary of the invention
The present invention is directed to the deficiency of above-mentioned prior art, and a kind of two-component acrylicester structural adhesive that provides.Another object of the present invention provides a kind of two-component acrylicester structural adhesive and preparation method.
The present invention has mainly solved problems such as the first fireballing deficiency of fixed bit speed slow, two component mixing after fixing of existing two-component acrylicester sizing agent.
In order to achieve the above object, the present invention is achieved in that a kind of bi-component acrylic structural adhesive, and the proportioning of host and solidifying agent is: 1: 1, host was made up of the following weight proportion raw material: monomer 30-50%; Elastomerics 0-18%, toughened resin 1-15%, base polyurethane prepolymer for use as 5-45%; γ-methacryloxypropyl trimethoxy silane 3-10%, N, N-dimethyl-p-toluidine 1-5%; Methylacrylic acid 1-15%, superoxide 0.5-4%, mineral filler 0-15%; Solidifying agent is made up of the following weight proportion raw material: monomer 30-70%, toughened resin 1-30%, elastomerics 0-30%, promotor 1-6%, mineral filler 0-15%, base polyurethane prepolymer for use as 1-70%; Described monomer is one or more mixing in isobornyl methacrylate, acryloyl morpholine, tetrahydrofuran ester, N-vinyl pyrrolidone, 1,6 hexanediol diacrylate, TEB 3K, Rocryl 400, the N hydroxymethyl acrylamide; Described elastomerics is one or more mixing in paracril, acrylic rubber, the ethylene-propylene rubber(EPR); Described toughened resin is one or more mixing among ABS, the PMMA; Superoxide is one or more mixing in hydroperoxide, ketone peroxide, the Lucidol; Described mineral filler is a white lake; Described promotor is by vanadic salts, or by the vanadic salts of 20-30%, the bisphenol A type epoxy resin of 70-80% mixes composition mutually.
Further, described vanadic salts is a Vanadium Pentoxide in FLAKES.
The preparation method of a kind of two-component acrylicester sizing agent provided by the invention is characterized in that comprising following process step: the preparation method of (1) host is: with said monomer, elastomerics; After toughened resin, base polyurethane prepolymer for use as, methylacrylic acid mix in proportion; Drop in the reaction kettle and stirred 10-15 hour, make it to become uniform liquid, add said gamma-methyl allyl acyloxypropyl trimethoxysilane when temperature returns to room temperature in proportion at 60-70 ℃; N, N-dimethyl-p-toluidine, superoxide; Stir 6-10h, obtain host.(2) preparation method of solidifying agent is: when promotor is two kinds of compositions, make according to the following steps: bisphenol A type epoxy resin is dropped in the reaction kettle, stirred 1-3 hour under the normal temperature, add vanadic salts and continue to stir 2 hours, make promotor; With said monomer, toughened resin, elastomerics, base polyurethane prepolymer for use as drops in the reaction kettle and stirred 10-15 hour at 60-70 ℃, makes it to become uniform liquid, returns to room temperature and adds promotor in proportion, and 4-8h is stirred in mineral filler, obtains solidifying agent.
Compared with present technology a kind of two-component acrylicester structural adhesive of the present invention and preparation method have substantive distinguishing features and the marked improvement that reality goes out: 1. speed was fast when this glue not only heated the location; And after this moment, glue mixed at normal temperatures the shelf-time still longer; Can reach more than 10 minutes, make things convenient for applying glue and shearing resistance high.2 preparation equipment, simple and easy, the environmental protection of technology, cost is low, and is applied widely.
Embodiment
In order better to understand and to implement, specify a kind of two-component acrylicester structural adhesive of the present invention and preparation method below in conjunction with embodiment.
Embodiment 1,
With 1,6 hexanediol diacrylate 20g, acryloyl morpholine 20g, base polyurethane prepolymer for use as 40g; After methylacrylic acid 3g mixes, drop in the reaction kettle and stirred 14 hours, make it to become uniform liquid at 62 ℃; When returning to room temperature, temperature adds gamma-methyl allyl acyloxypropyl trimethoxysilane 5g, N, N-dimethyl-p-toluidine 1.5g; Isopropyl benzene hydroperoxide 2g stirs 9h, obtains host.
Cobalt iso-octoate 2.1g or bisphenol A type epoxy resin 7.4g are dropped in the reaction kettle, and normal temperature stirred 1.2 hours down, dropped into Vanadium Pentoxide in FLAKES salt 2.1g, continued to stir 2 hours, made promotor;
With TEB 3K 60g, ethylene-propylene rubber(EPR) 25g, ABS 10g; Base polyurethane prepolymer for use as 25g drops in the reaction kettle and stirred 11 hours at 63 ℃, makes it to become uniform liquid, returns to room temperature and adds the above-mentioned promotor 1.5g that makes; White lake 10g stirs 5h, obtains solidifying agent.
Embodiment 2,
With TEB 3K 10g, acryloyl morpholine 20g, N hydroxymethyl acrylamide 15g, ABS10g; Base polyurethane prepolymer for use as 20g after methylacrylic acid 15g mixes, drops in the reaction kettle and stirred 11 hours at 68 ℃, makes it to become uniform liquid; When returning to room temperature, temperature adds gamma-methyl allyl acyloxypropyl trimethoxysilane 8g, N, N-dimethyl-p-toluidine 1.2g; Isopropyl benzene hydroperoxide 1g stirs 8.1h, obtains host.
Bisphenol A type epoxy resin 7.3 is dropped in the reaction kettle, and normal temperature stirred 1.1 hours down, dropped into Vanadium Pentoxide in FLAKES salt 2.7g, continued to stir 2 hours, made promotor; With TEB 3K 68g, ethylene-propylene rubber(EPR) 28g, base polyurethane prepolymer for use as 15g drops in the reaction kettle and stirred 13 hours at 67 ℃; Make it to become uniform liquid, return to room temperature and add said process gained promotor 1.5g, white lake 13g; Stir 6h, obtain solidifying agent.
Embodiment 3,
With acryloyl morpholine 20g, N hydroxymethyl acrylamide 20g, PMMA10g, base polyurethane prepolymer for use as 40g; After methylacrylic acid 3g mixes, drop in the reaction kettle and stirred 7.4 hours, make it to become uniform liquid at 63 ℃; When returning to room temperature, temperature adds gamma-methyl allyl acyloxypropyl trimethoxysilane 5g, N, N-dimethyl-p-toluidine 1.5g; Isopropyl benzene hydroperoxide 1.5g stirs 6.9h, obtains host.
With TEB 3K 60g, ABS 27g, base polyurethane prepolymer for use as 5g drop in the reaction kettle and stirred 7.2 hours at 63.5 ℃, make it to become uniform liquid, return to room temperature and add Vanadium Pentoxide in FLAKES 2g in proportion, stir 6.5h, obtain solidifying agent.
Embodiment 4,
With tetrahydrofuran ester 30g, acryloyl morpholine 20g, base polyurethane prepolymer for use as 45g; After methylacrylic acid 15g mixes, drop in the reaction kettle and stirred 15 hours, make it to become uniform liquid at 70 ℃; When returning to room temperature, temperature adds gamma-methyl allyl acyloxypropyl trimethoxysilane 10g, N, N-dimethyl-p-toluidine 5g; Lucidol 4g stirs 10h, obtains host.
Bisphenol A type epoxy resin 70g is dropped in the reaction kettle, and normal temperature stirred 1 hour down, dropped into Vanadium Pentoxide in FLAKES 20g, continued to stir 2 hours, made promotor;
With TEB 3K 70g, ABS 30g, base polyurethane prepolymer for use as 70g drop in the reaction kettle and stirred 15 hours at 60 ℃, make it to become uniform liquid, return to room temperature and add the above-mentioned short Vanadium Pentoxide in FLAKES 6g that makes, and stir 8h, obtain solidifying agent.
Embodiment 5,
With tetrahydrofuran ester 30g, acryloyl morpholine 20g, base polyurethane prepolymer for use as 45g; After methylacrylic acid 15g mixes, drop in the reaction kettle and stirred 15 hours, make it to become uniform liquid at 70 ℃; When returning to room temperature, temperature adds gamma-methyl allyl acyloxypropyl trimethoxysilane 10g, N, N-dimethyl-p-toluidine 5g; Lucidol 4g stirs 10h, obtains host.
Bisphenol A type epoxy resin 80g is dropped in the reaction kettle, and normal temperature stirred 3 hours down, dropped into Vanadium Pentoxide in FLAKES 30g, continued to stir 2 hours, made promotor;
With TEB 3K 70g, ABS 30g, base polyurethane prepolymer for use as 70g drop in the reaction kettle and stirred 15 hours at 670 ℃, make it to become uniform liquid, return to room temperature and add the above-mentioned short Vanadium Pentoxide in FLAKES 6g that makes, and stir 8h, obtain solidifying agent.
Performance test:
Test result is seen table 1.
Figure BSA00000721444600051
Figure BSA00000721444600061
Table 1
1. stability: in two component packing tubes of will gained sizing agent among above-mentioned 6 embodiment packing into, placement naturally, gel time appears in mensuration.
2. shearing resistance: press GB/T7124-1986 and carry out
3. just between busy hour fixed: aluminium flake is put into 60 ℃/80 ℃ baking oven preheatings, and the sizing agent that two components are mixed is coated on the aluminium flake of preheating, and the aluminium flake shearing resistance reaches the required time greater than 0.2MPa in baking oven.
As above shown in the table, this glue reaches the time required greater than 0.2MPa 80 ℃ and shearing resistance and can reach within the scope of 35-45S.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any pro forma restriction, every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.

Claims (3)

1. two-component acrylicester structural adhesive, the proportioning of host and solidifying agent is: 1: 1, it is characterized by: host is made up of the raw material of following weight parts: monomer 30-50%; Elastomerics 0-18%, toughened resin 1-15%, base polyurethane prepolymer for use as 5-45%; γ-methacryloxypropyl trimethoxy silane 3-10%, N, N-dimethyl-p-toluidine 1-5%; Methylacrylic acid 1-15%, superoxide 0.5-4%, mineral filler 0-15%; Solidifying agent is made up of the raw material of following weight parts: monomer 30-70%, toughened resin 1-30%, elastomerics 0-30%, promotor 1-6%, mineral filler 0-15%, base polyurethane prepolymer for use as 1-70%; Described monomer is one or more mixing in isobornyl methacrylate, acryloyl morpholine, tetrahydrofuran ester, N-vinyl pyrrolidone, 1,6 hexanediol diacrylate, TEB 3K, Rocryl 400, the N hydroxymethyl acrylamide; Described elastomerics is one or more mixing in paracril, acrylic rubber, the ethylene-propylene rubber(EPR); Described toughened resin is one or more mixing among ABS, the PMMA; Superoxide is one or more mixing in hydroperoxide, ketone peroxide, the Lucidol; Described mineral filler is a white lake; Described promotor is vanadic salts, or by the vanadic salts of 20-30%, the bisphenol A type epoxy resin of 70-80% mixes composition mutually.
2. a kind of two-component acrylicester structural adhesive according to claim 1, described vanadic salts is a Vanadium Pentoxide in FLAKES.
3. the preparation method who is used for the described a kind of two-component acrylicester structural adhesive of claim 1 is characterized in that comprising following process step:
(1) preparation method of host is: with said monomer, elastomerics, toughened resin, base polyurethane prepolymer for use as; After methylacrylic acid mixes in proportion, drop in the reaction kettle and stirred 10-15 hour, make it to become uniform liquid at 60-70 ℃; When returning to room temperature, temperature adds said gamma-methyl allyl acyloxypropyl trimethoxysilane in proportion, N, N-dimethyl-p-toluidine; Superoxide stirs 6-10h, obtains host.
(2) preparation method of solidifying agent is: when promotor is two kinds of compositions, make according to the following steps: bisphenol A type epoxy resin is dropped in the reaction kettle, stirred 1-3 hour under the normal temperature, add vanadic salts and continue to stir 2 hours, make promotor; With said monomer, toughened resin, elastomerics, base polyurethane prepolymer for use as drops in the reaction kettle and stirred 10-15 hour at 60-70 ℃, makes it to become uniform liquid, returns to room temperature and adds promotor in proportion, and 4-8h is stirred in mineral filler, obtains solidifying agent.
CN2012101610388A 2012-05-23 2012-05-23 Bi-component acrylic ester structure adhesive and preparation method thereof Pending CN102746796A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104327752A (en) * 2014-10-15 2015-02-04 烟台德邦科技有限公司 Acrylic acid structural adhesive with good weatherability and stability
CN104356964A (en) * 2014-12-02 2015-02-18 北京天山新材料技术有限公司 Preparation of low-odor and environment-friendly acrylate structural glue
WO2017035863A1 (en) * 2015-09-02 2017-03-09 刘洋 Adhesive for metal part
CN109593311A (en) * 2017-09-30 2019-04-09 比亚迪股份有限公司 Acrylate resin composition and acrylate injection-molded product and its preparation method and application
CN111040720A (en) * 2019-12-19 2020-04-21 烟台德邦科技有限公司 Rapid-positioning bi-component polyurethane adhesive and preparation method thereof
JP2021024910A (en) * 2019-08-01 2021-02-22 昭和電工マテリアルズ株式会社 Adhesive set and method for producing structure

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1295106A (en) * 1999-11-08 2001-05-16 成都正光科技股份有限公司 Structural acrylate glue
CN101392153A (en) * 2008-09-28 2009-03-25 广东恒大新材料科技有限公司 Bi-component acrylic ester adhesive
CN102382579A (en) * 2011-06-21 2012-03-21 烟台德邦科技有限公司 Acrylic ester structural adhesive having high intensity and high thixotropy and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1295106A (en) * 1999-11-08 2001-05-16 成都正光科技股份有限公司 Structural acrylate glue
CN101392153A (en) * 2008-09-28 2009-03-25 广东恒大新材料科技有限公司 Bi-component acrylic ester adhesive
CN102382579A (en) * 2011-06-21 2012-03-21 烟台德邦科技有限公司 Acrylic ester structural adhesive having high intensity and high thixotropy and preparation method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104327752A (en) * 2014-10-15 2015-02-04 烟台德邦科技有限公司 Acrylic acid structural adhesive with good weatherability and stability
CN104327752B (en) * 2014-10-15 2016-04-27 烟台德邦科技有限公司 A kind of weathering resistance and the acrylic acid structure glue had good stability
CN104356964A (en) * 2014-12-02 2015-02-18 北京天山新材料技术有限公司 Preparation of low-odor and environment-friendly acrylate structural glue
WO2017035863A1 (en) * 2015-09-02 2017-03-09 刘洋 Adhesive for metal part
CN109593311A (en) * 2017-09-30 2019-04-09 比亚迪股份有限公司 Acrylate resin composition and acrylate injection-molded product and its preparation method and application
CN109593311B (en) * 2017-09-30 2021-05-14 比亚迪股份有限公司 Acrylate resin composition, acrylate resin injection molding product, preparation method and application thereof
JP2021024910A (en) * 2019-08-01 2021-02-22 昭和電工マテリアルズ株式会社 Adhesive set and method for producing structure
JP7338303B2 (en) 2019-08-01 2023-09-05 株式会社レゾナック ADHESIVE SET AND STRUCTURE MANUFACTURING METHOD
CN111040720A (en) * 2019-12-19 2020-04-21 烟台德邦科技有限公司 Rapid-positioning bi-component polyurethane adhesive and preparation method thereof

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