CN102604547A - High-temperature resistant anaerobic locking glue and preparation method thereof - Google Patents
High-temperature resistant anaerobic locking glue and preparation method thereof Download PDFInfo
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- CN102604547A CN102604547A CN2012100412873A CN201210041287A CN102604547A CN 102604547 A CN102604547 A CN 102604547A CN 2012100412873 A CN2012100412873 A CN 2012100412873A CN 201210041287 A CN201210041287 A CN 201210041287A CN 102604547 A CN102604547 A CN 102604547A
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Abstract
The invention relates to a high-temperature resistant anaerobic locking glue and a preparation method of the high-temperature resistant anaerobic locking glue. The anaerobic locking glue comprises 45 parts of (2) ethoxylated bisphenol A dimethacrylate, 20 parts of hydroxypropyl methacrylate, 15 parts of boric acid, 12.39 parts of bisphenol A fumaric acid polyester, 3 parts of fumed silica, 0.8 part of benzoic hydrazine, 0.6 part of o-benzene sulfonyl imine, 1.0 part of ethylenediamine tetraacetic acid disodium salt, 2.0 parts of cumene hydroperoxide, 0.2 part of fast red, and 0.01 part of para-benzoquinone. The anaerobic locking glue can be used for a short time at the temperature blow 230 DEG C and a long time at the temperature above 200 DEG C. The thermal aging resistance of the anaerobic locking glue at 230 DEG C is improved significantly. The anaerobic locking glue has a wide range of application and overcomes the defects that the existing ordinary anaerobic glue can not adapt to the high-temperature working condition.
Description
Technical field
The present invention relates to anaerobic adhesive, especially relate to resistant to elevated temperatures anaerobic glue of ability that is fit to the occasion of the certain locking of needs moment under the high temperature and preparation method thereof.This anaerobic glue can be used for each industrial circles such as automobile industry, aviation, military project, universal machine, transportation machinery, oil field, industry and civilian pipeline, mould manufacturing.
Background technology
Along with the development of modern science and technology, anaerobic adhesive has played more and more important effect in people's life.Especially in automobile industry, the track traffic industry, anaerobic glue has replaced traditional locking seal means, has not only guaranteed quality, has also reduced cost, has made things convenient for workman's operation.But present anaerobic glue major part belongs to traditional anaerobic glue; Character according to general chemical; Generally can heatproof to 150 ℃; Also there is the utmost point discrete can heatproof to 230 ℃, but life-time service at high temperature, must be at high temperature but the demand of the certain locking moment of needs simultaneously so can't satisfy some occasions.Maybe be such as temperature in high-temperature boiler up to 200 ℃, screw wherein need be fixed, and common just can not satisfy this requirement.Just need a kind of anaerobic glue that can at high temperature use and can satisfy locking moment for a long time this moment; Prior art mainly is to reach resistant to elevated temperatures purpose through adding stable on heating mineral filler.And the system of general mineral filler and anaerobic glue is not too compatible, so need to select appropriate filler to achieve the goal.Before this, have the people to reach resistant to elevated temperatures purpose, but the product that this kind method makes can't satisfy the requirement of long-term locking under higher temperature through the material that adds polyimide; Some operating modes need anaerobic glue at high temperature to have certain locking moment for a long time at present; And the long-term heat aging property of common anaerobic glue is relatively poor; General heatproof to 150 ℃, and in the words of 150 ℃ of following life-time service also lost strength slowly, promptly heat aging performance is relatively poor.The high-temperature plastic that has also can only be that short-term is anti-to 230 ℃, can't be under this temperature life-time service, can't satisfy the use under some special operation conditions.
Summary of the invention
The objective of the invention is to produce in order to solve an above-mentioned difficult problem; Cooperate other monomers, initiator, promotor, tensio-active agent and stablizer to make the anaerobic glue of high thermal resistance through adding a certain amount of boric acid; Solving common anaerobic glue can not resistant to elevated temperatures problem; The anaerobic glue heatproof can be reached more than 230 ℃, and have secular heat aging property;
In order to realize the object of the invention.Propose a kind of high temperature resistant anaerobism locking glue, mark is composed of the following components by weight for this anaerobism locking glue:
Methacrylate monomers 40-85 part
Thickening material 5-20 part
Heat-resisting additive 10-30 part thixotropic agent 1-5 part
Promotor 0.1-3 part
Secondary accelerator 0.1-5 part
Initiator 1-10 part
Stopper 0.005-0.1 part
Sequestrant 0.01-0.2 part;
Said methacrylate monomers is TEB 3K, methacrylic ester ethyl ester, cyclohexyl methacrylate, (2) ethoxyquin bisphenol a dimethacrylate, 1; 3-butylene glycol dimethacrylate, 1; 4-butylene glycol dimethacrylate, isobornyl methacrylate, IBOA, tert-butylcyclohexyl methacrylic ester, 1; The mixture of one or more in 6-hexanediol dimethacrylate, 1,6 hexanediol diacrylate, methylacrylic acid tetrahydrofuran ester, the vinylformic acid tetrahydrofuran ester.In addition, also can add Rocryl 400, Rocryl 410, tetraethylene-glycol dimethacrylate, Tri Ethyleneglycol dimethacrylate, polyoxyethylene glycol (200) dimethacrylate or three (2-hydroxyethyl) isocyanuric acid triacrylate monomer in the anaerobic glue of the present invention;
Said thickening material is one or more the mixture in polymethylmethacrylate, polyethyl methacrylate, poly-n-butyl methacrylate, dihydroxyphenyl propane fumarate polyester, Yodo Sol VC 400, the polyvinyl butyral acetal;
Said heat-resisting additive is chosen to be boric acid;
Said promotor is N, N '-dimethyl-p-toluidine, N, N '-dimethyl-Ortho Toluidine, N, the mixture of one or more in N '-diethyl-p-tlouidine, tri-n-butylamine, triethylamine, trolamine, ferrocene, pyrodin and the benzoyl hydrazine;
Said thixotropic agent is an aerosil;
Said secondary accelerator is one or more the mixture in benzoic sulfimide, xitix, methylacrylic acid, the vinylformic acid;
Said initiator is a kind of in isopropyl benzene hydroperoxide, tertbutyl peroxide, the peroxidized t-butyl perbenzoate;
Said stopper is one or more mixtures in Resorcinol, para benzoquinone, naphthoquinones, the p methoxy phenol;
Said sequestrant is tetrasodium salt of EDTA or disodium EDTA;
Said anaerobism locking glue also comprises other auxiliary agents of 0.01-1 part, and said other auxiliary agents are dyestuff or pigment;
As an embodiment, said anaerobism locking glue mark by weight is made up of following concrete component:
(2) the ethoxyquin bisphenol a dimethacrylate is 45 parts
20 parts of Rocryl 410s
15 parts of boric acid
12.39 parts of dihydroxyphenyl propane fumarate polyesters
3 parts of aerosils
0.8 part of benzoyl hydrazine
0.6 part of adjacent benzenesulfonimide
1.0 parts of disodium EDTAs
2.0 parts of isopropyl benzene hydroperoxides
Red 0.2 part of sun-proof
0.01 part of para benzoquinone.
The present invention also proposes a kind of preparation method of high temperature resistant anaerobism locking glue, and said method comprises step:
1) (2) ethoxyquin bisphenol a dimethacrylate, Rocryl 410 and disodium EDTA are added in the reaction flask, stirred 2 hours down at 25 ~ 40 ℃;
2) add dihydroxyphenyl propane fumarate polyester, boric acid, benzoyl hydrazine, adjacent benzenesulfonimide, sun-proof is red and para benzoquinone, adds aerosil again and is stirred to whole dissolvings, is cooled to room temperature;
3) add isopropyl benzene hydroperoxide, stirring gets product;
With compared with techniques in the past, the present invention can use 230 ℃ of following short-terms, at life-time service more than 200 ℃; Through test; The heat-resistant aging of this product under 230 ℃ has tangible raising, is higher than happy safe 272 the heat-resistant aging of rival, has wide application field; Satisfied the demand that present common anaerobic glue can't adapt to worst hot case, especially common anaerobic glue can not satisfy the weak point of the condition of locking under the high temperature.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, to further explain of the present invention;
Prepare a kind of fire resistant anaerobic adhesive; Its composition contains (2) ethoxyquin bisphenol a dimethacrylate, Rocryl 410, boric acid, dihydroxyphenyl propane fumarate polyester, benzoyl hydrazine, disodium EDTA, adjacent benzenesulfonimide and isopropyl benzene hydroperoxide, red, the para benzoquinone of sun-proof, and the parts by weight proportioning of said composition is following:
(2) the ethoxyquin bisphenol a dimethacrylate is 45 parts
20 parts of Rocryl 410s
15 parts of boric acid
12.39 parts of dihydroxyphenyl propane fumarate polyesters
3 parts of aerosils
0.8 part of benzoyl hydrazine
0.6 part of adjacent benzenesulfonimide
1.0 parts of disodium EDTAs
2.0 parts of isopropyl benzene hydroperoxides
Red 0.2 part of sun-proof
0.01 part of para benzoquinone
During preparation; Earlier will (2) ethoxyquin bisphenol a dimethacrylate, Rocryl 410 and disodium EDTA add in the reaction flask, 25 ~ 40 ℃ of stirrings 2 hours down, adds dihydroxyphenyl propane fumarate polyester, boric acid, benzoyl hydrazine, adjacent benzenesulfonimide again, sun-proof is red and para benzoquinone; Add aerosil again and be stirred to whole dissolvings; Be cooled to room temperature, add isopropyl benzene hydroperoxide at last again, stirring gets product;
Anaerobism locking glue by present method makes is compared with happy safe common anaerobic glue 262 and high-temperature plastic 272, and its performance is relatively like following table:
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further detailed description, and institute it should be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. a high temperature resistant anaerobism locking glue is characterized in that, mark is composed of the following components by weight for this anaerobism locking glue:
Methacrylate monomers 40-85 part
Thickening material 5-20 part
Heat-resisting additive 10-30 part thixotropic agent 1-5 part
Promotor 0.1-3 part
Secondary accelerator 0.1-5 part
Initiator 1-10 part
Stopper 0.005-0.1 part
Sequestrant 0.01-0.2 part;
Said methacrylate monomers is TEB 3K, methacrylic ester ethyl ester, cyclohexyl methacrylate, (2) ethoxyquin bisphenol a dimethacrylate, 1; 3-butylene glycol dimethacrylate, 1; 4-butylene glycol dimethacrylate, isobornyl methacrylate, IBOA, tert-butylcyclohexyl methacrylic ester, 1; The mixture of one or more in 6-hexanediol dimethacrylate, 1,6 hexanediol diacrylate, methylacrylic acid tetrahydrofuran ester, the vinylformic acid tetrahydrofuran ester; In addition, also can add Rocryl 400, Rocryl 410, tetraethylene-glycol dimethacrylate, Tri Ethyleneglycol dimethacrylate, polyoxyethylene glycol (200) dimethacrylate or three (2-hydroxyethyl) isocyanuric acid triacrylate monomer in the anaerobic glue of the present invention;
Said thickening material is one or more the mixture in polymethylmethacrylate, polyethyl methacrylate, poly-n-butyl methacrylate, dihydroxyphenyl propane fumarate polyester, Yodo Sol VC 400, the polyvinyl butyral acetal;
Said heat-resisting additive is chosen to be boric acid;
Said promotor is N, N '-dimethyl-p-toluidine, N, N '-dimethyl-Ortho Toluidine, N, the mixture of one or more in N '-diethyl-p-tlouidine, tri-n-butylamine, triethylamine, trolamine, ferrocene, pyrodin and the benzoyl hydrazine;
Said thixotropic agent is an aerosil;
Said secondary accelerator is one or more the mixture in benzoic sulfimide, xitix, methylacrylic acid, the vinylformic acid;
Said initiator is a kind of in isopropyl benzene hydroperoxide, tertbutyl peroxide, the peroxidized t-butyl perbenzoate;
Said stopper is one or more mixtures in Resorcinol, para benzoquinone, naphthoquinones, the p methoxy phenol;
Said sequestrant is tetrasodium salt of EDTA or disodium EDTA.
2. anaerobism locking glue according to claim 1 is characterized in that said anaerobism locking glue also comprises other auxiliary agents of 0.01-1 part, and said other auxiliary agents are dyestuff or pigment.
3.
.According to the described anaerobism locking of claim 1-2 glue, it is characterized in that mark is composed of the following components by weight for said anaerobism locking glue:
(2) the ethoxyquin bisphenol a dimethacrylate is 45 parts
20 parts of Rocryl 410s
15 parts of boric acid
12.39 parts of dihydroxyphenyl propane fumarate polyesters
3 parts of aerosils
0.8 part of benzoyl hydrazine
0.6 part of adjacent benzenesulfonimide
1.0 parts of disodium EDTAs
2.0 parts of isopropyl benzene hydroperoxides
Red 0.2 part of sun-proof
0.01 part of para benzoquinone.
4. preparation is characterized in that like the preparation method of the said high temperature resistant anaerobism locking glue of claim 1-3 said method comprises step:
1) (2) ethoxyquin bisphenol a dimethacrylate, Rocryl 410 and disodium EDTA are added in the reaction flask, stirred 2 hours down at 25 ~ 40 ℃;
2) add dihydroxyphenyl propane fumarate polyester, boric acid, benzoyl hydrazine, adjacent benzenesulfonimide, sun-proof is red and para benzoquinone, adds aerosil again and is stirred to whole dissolvings, is cooled to room temperature;
3) add isopropyl benzene hydroperoxide, stirring gets product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012100412873A CN102604547A (en) | 2012-02-23 | 2012-02-23 | High-temperature resistant anaerobic locking glue and preparation method thereof |
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| CN2012100412873A CN102604547A (en) | 2012-02-23 | 2012-02-23 | High-temperature resistant anaerobic locking glue and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104650745A (en) * | 2014-06-12 | 2015-05-27 | 徐饶春 | Anaerobic adhesive and preparation method thereof |
| CN109852303A (en) * | 2018-12-29 | 2019-06-07 | 宁波大榭开发区综研化学有限公司 | A kind of high temperature resistant double faced adhesive tape and preparation method |
| CN109852297A (en) * | 2019-03-15 | 2019-06-07 | 湖南辰砾新材料有限公司 | A kind of anaerobic type waterproof sealing structure glue for building |
| CN111777953A (en) * | 2020-07-31 | 2020-10-16 | 黑龙江省科学院石油化学研究院 | Thread locking anaerobic adhesive and preparation method thereof |
| CN115433524A (en) * | 2022-10-11 | 2022-12-06 | 武汉中科先进材料科技有限公司 | Thread locking anaerobic adhesive and preparation method thereof |
| GB2622079A (en) * | 2022-09-01 | 2024-03-06 | Henkel Ag & Co Kgaa | Anaerobically curable compositions |
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| JPH04117474A (en) * | 1990-01-08 | 1992-04-17 | Okura Ind Co Ltd | Anaerobic adhesive |
| CN1226589A (en) * | 1998-02-19 | 1999-08-25 | 梁义勋 | Preparation of mono-component anaerobic adhesive for fastening screws and sealing flat surfaces |
| CN101531876A (en) * | 2009-04-20 | 2009-09-16 | 北京天山新材料技术有限责任公司 | Superstrength anaerbic adhesive capable of fast curing under low temperature and preparation method |
| CN101705071A (en) * | 2009-10-08 | 2010-05-12 | 广东三和化工科技有限公司 | High-temperature-resistant structure anaerobic adhesive |
| CN101743260A (en) * | 2007-07-16 | 2010-06-16 | 汉高公司 | thermally resistant anaerobically curable compositions |
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2012
- 2012-02-23 CN CN2012100412873A patent/CN102604547A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04117474A (en) * | 1990-01-08 | 1992-04-17 | Okura Ind Co Ltd | Anaerobic adhesive |
| CN1226589A (en) * | 1998-02-19 | 1999-08-25 | 梁义勋 | Preparation of mono-component anaerobic adhesive for fastening screws and sealing flat surfaces |
| CN101743260A (en) * | 2007-07-16 | 2010-06-16 | 汉高公司 | thermally resistant anaerobically curable compositions |
| CN101531876A (en) * | 2009-04-20 | 2009-09-16 | 北京天山新材料技术有限责任公司 | Superstrength anaerbic adhesive capable of fast curing under low temperature and preparation method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104650745A (en) * | 2014-06-12 | 2015-05-27 | 徐饶春 | Anaerobic adhesive and preparation method thereof |
| CN109852303A (en) * | 2018-12-29 | 2019-06-07 | 宁波大榭开发区综研化学有限公司 | A kind of high temperature resistant double faced adhesive tape and preparation method |
| CN109852297A (en) * | 2019-03-15 | 2019-06-07 | 湖南辰砾新材料有限公司 | A kind of anaerobic type waterproof sealing structure glue for building |
| CN111777953A (en) * | 2020-07-31 | 2020-10-16 | 黑龙江省科学院石油化学研究院 | Thread locking anaerobic adhesive and preparation method thereof |
| CN111777953B (en) * | 2020-07-31 | 2021-10-29 | 黑龙江省科学院石油化学研究院 | Thread locking anaerobic adhesive and preparation method thereof |
| GB2622079A (en) * | 2022-09-01 | 2024-03-06 | Henkel Ag & Co Kgaa | Anaerobically curable compositions |
| WO2024046703A1 (en) * | 2022-09-01 | 2024-03-07 | Henkel Ag & Co. Kgaa | Anaerobically curable compositions |
| CN115433524A (en) * | 2022-10-11 | 2022-12-06 | 武汉中科先进材料科技有限公司 | Thread locking anaerobic adhesive and preparation method thereof |
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Application publication date: 20120725 |