CN100383210C - Low temperature detachable anaerobic adhesive and method for preparing the same - Google Patents
Low temperature detachable anaerobic adhesive and method for preparing the same Download PDFInfo
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- CN100383210C CN100383210C CNB2005101273346A CN200510127334A CN100383210C CN 100383210 C CN100383210 C CN 100383210C CN B2005101273346 A CNB2005101273346 A CN B2005101273346A CN 200510127334 A CN200510127334 A CN 200510127334A CN 100383210 C CN100383210 C CN 100383210C
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Abstract
The present invention relates to low temperature detachable anaerobic adhesive and a preparation method thereof, particularly to detachable anaerobic adhesive and a preparation method thereof. The present invention solves the problems of the existing anaerobic adhesive that the maintenance is poor, components are difficult to detach, material without high temperature resistance and a locking piece with large thread diameter are difficult to detach, and the adhesion reliability of the anaerobic adhesive is reduced. A product of the present invention is prepared by following steps: A.(by weight) 50 to 95 portions of methacrylic acid diester monomer and 0.01 to 2 portions of stabilizing agent are taken and are mixed, stirred and dissloved at temperature of 45 to 55 DEG C; B. 0.1 to 5 portions of accelerating agent and 0.1 to 5 portions of o-benzoic sulfimide are added into the mixture of the step A, and the formed mixture is stirred; C. 10 to 50 portions of unsaturated polyester and 5 to 50 portions of modifying agent and 0.1 to 5 portions of silicon dioxide are added into the mixture of the step B and are dissolved, and the formed mixture is cooled to room temperature. D. 1 to 10 portions of oxide is added into the mixture of the step C, and the formed mixture is uniformly mixed. The anaerobic adhesive of the present invention has the characteristics of convenient operation time at maintenance time, easy component detaching operation, small influence for adhesion strength, low cost and high effectiveness.
Description
Technical field
The present invention relates to detachable anaerobic adhesive and preparation method thereof.
Background technology
Before chemistry locking and seal gum technology occur, people once adopted multiple mechanical means to be used for locking thread, these methods all are to increase component, it is basic improving working accuracy, the result causes the increase of cost, moreover still can't fundamentally prevent looseningly, more can't avoid the seepage at screw thread place.And the birth of anaerobic adhesive has solved an above-mentioned difficult problem.But behind the employing adhesive bonding technique, when product keeps in repair, screw element and flange components dismounting difficulty, particularly high strength anaerobic glue and major diameter screw fastening firmware at room temperature can't be dismantled.At present, the main heat method for dismounting that adopts, heating will reach more than 200 ℃, will reach 300～400 ℃ of ability dismountings sometimes, and some parts is subjected to the restriction (as cast aluminium, magnesium alloy) of material etc. can't heat, has just occurred keeping in repair and new problem such as dismounting.At present, the bonding strengths that adopt the method for adding softening agent to reduce anaerobic glue make it more quick detachable more on the market.1974, the famous in the world Loctite.Co of anaerobic glue company has delivered the patent of detachable anaerobic adhesive, (US3794610) this patent adopts polyester plasticizer that the methacrylic acid diester is carried out modification, prepare easily detachable middle low strength anaerobic glue, this method has satisfied the detachable performance of anaerobic glue to a certain extent.But, on using, be very limited because the reduction of intensity can make the bonding reliability decrease of anaerobic glue.
Summary of the invention
The present invention is poor in order to solve existing anaerobic glue serviceability, parts dismounting difficulty, the problem that the high strength anaerobic glue of non-refractory material and major diameter screw fastening firmware can't be dismantled and the bonding reliability of middle low strength anaerobic glue reduces particularly, a kind of low-temperature heat detachable anaerobic adhesive and preparation method thereof now is provided, and the technical scheme that addresses the above problem is as follows:
Low temperature detachable anaerobic adhesive of the present invention is made for 1～10 part by 50～95 parts of methacrylic acid diester monomers, 10～50 parts of unsaturated polyesters, 0.1～5 part of promotor, 0.1～5 part of adjacent benzenesulfonimide, 0.01～2 part of stablizer, 5～50 parts of thermal softening properties-correcting agent, 0.1～5 part of aerosil and organo-peroxide by weight.
The preparation method of a kind of low temperature detachable anaerobic adhesive of the present invention, this method is realized by the following step:
A, get 0.01～2 part of 50～95 parts of methacrylic acid diester monomer, stablizer earlier by weight and mix stirring, dissolving, stirred 30～120 minutes at 45～55 ℃;
B, in steps A, add promotor 0.1～5 weight part and adjacent benzenesulfonimide 0.1～5 weight part is stirred to molten entirely;
C, in step B, add unsaturated polyester 10～50 weight parts, thermal softening properties-correcting agent 5～50 weight parts and aerosil 0.1～5 weight part again, after treating to dissolve fully, be cooled to room temperature;
D, in step C, add organo-peroxide 1～10 weight part again and stir, promptly be prepared into low temperature detachable anaerobic adhesive.
Low temperature detachable anaerobic adhesive of the present invention is when parts for maintenance, screw thread and flange components are dismantled smoothly, also be applicable to the dismounting of high strength anaerobic glue and major diameter screw fastening firmware, wracking moment and dismounting force moment reduce by 50～80% after heating, the bonding strength of the reduction explanation anaerobic glue of moment descends, and the anaerobic glue that adds properties-correcting agent is little to the influence of anaerobic glue bonding strength under use temperature, the bonding strength and the use properties of anaerobic glue have been guaranteed, it is low also to have cost, the characteristics of high efficiency.
Embodiment
Embodiment one: present embodiment is made for 1～10 part by 50～95 parts of methacrylic acid diester monomers, 10～50 parts of unsaturated polyesters, 0.1～5 part of promotor, 0.1～5 part of adjacent benzenesulfonimide, 0.01～2 part of stablizer, 5～50 parts of thermal softening properties-correcting agent, 0.1～5 part of aerosil and organo-peroxide by weight.
Above-mentioned methacrylic acid diester monomer is selected glycolmethacrylate, multicondensed ethylene glycol double methyl methacrylate, ethoxyquin dihydroxyphenyl propane dimethyl allene acid diester, trimethylolpropane trimethacrylate, Rocryl 410 or multiple epoxy acrylate monomer for use;
Unsaturated polyester is selected the fumaric acid bisphenol a resin for use;
Promotor is selected pyrodin, benzoyl hydrazine for use, also can select N for use, N-dimethyl-p-toluidine, N, N-Diethyl Aniline or triethylamine;
Stablizer is selected oxalic acid, ethylenediamine tetraacetic acid (EDTA) (EDTA), o-aminophenol, oxine, many pyridine compounds, phosphoric acid derivatives for use or with dihydroxy-benzene, benzoquinones, naphthoquinones, anthraquinone stopper;
Thermal softening properties-correcting agent can be selected rosin, maleated rosin, polymerized rosin, various heat resistance modified rosin, terpenes, rosin ester, nylon powder, polyethylene powders, polypropylene powder or polyvinyl chloride powder for use.
Unsaturated polyester is the intensity that is used for regulating anaerobic glue.
Properties-correcting agent is the heat resistance that is used for regulating anaerobic glue, and properties-correcting agent has the thermal softening performance, and the anaerobic glue bond can be dismantled under 80～200 ℃ temperature environment smoothly.Its detachable temperature can be regulated by the properties-correcting agent that adds different thermal softening temperature.Selecting for use on the use temperature of anaerobic glue of properties-correcting agent decided, and it is more suitable generally to select for use softening temperature to be higher than the properties-correcting agent of 10～30 ℃ of use temperatures.When temperature 〉=thermal softening temperature, the thermal softening properties-correcting agent in the anaerobic glue takes place softening, and bonding strength is sharply descended, and is beneficial to dismounting; When temperature was lower than softening temperature, properties-correcting agent was little to the bonding strength influence of anaerobic glue, thereby had guaranteed the bonding strength of anaerobic glue.
Embodiment two: it is made for 1～5 part by 50～70 parts of methacrylic acid diester monomers, 10～30 parts of unsaturated polyesters, 0.1～2.5 part of promotor, 0.1～2.5 part of adjacent benzenesulfonimide, 0.01～1 part of stablizer, 5～25 parts of thermal softening properties-correcting agent, 0.1～2.5 part of aerosil and organo-peroxide present embodiment by weight.
Embodiment three: it is made for 6～10 parts by 71～90 parts of methacrylic acid diester monomers, 31～50 parts of unsaturated polyesters, 2.6～5 parts of promotor, 2.6～5 parts of adjacent benzenesulfonimides, 1.1～2 parts of stablizers, 26～50 parts of thermal softening properties-correcting agent, 2.6～5 parts of aerosils and organo-peroxide present embodiment by weight.
Embodiment four: the preparation method of a kind of low temperature detachable anaerobic adhesive of present embodiment, this method is realized by the following step:
A, get 0.01～2 part of 50～95 parts of methacrylic acid diester monomer, stablizer earlier by weight and carry out mechanical stirring, dissolving, stirred 30～120 minutes 45～55 ℃ of mixing;
B, add promotor 0.1～5 weight part and adjacent benzenesulfonimide 0.1～5 weight part be stirred to moltenly entirely in steps A, churning time is 30～60 minutes;
C, in step B, add unsaturated polyester 10～50 weight parts, thermal softening properties-correcting agent 5～50 weight parts and aerosil 0.1～5 weight part again, after treating to dissolve fully, be cooled to room temperature;
D, add organo-peroxide 1～10 weight part again in step C and stir, churning time is 30～60 minutes, promptly is prepared into low temperature detachable anaerobic adhesive.
Embodiment five: present embodiment is got 0.02 part of oxalic acid by weight and is joined in 70 parts of Triethylene glycol dimethacrylate monomers and stir, be warming up to 45 ℃ and make its dissolving, add 1 part of pyrodin again and 1.5 parts of adjacent benzenesulfonimides are stirred to molten entirely, and then add 40 parts of fumaric acid bisphenol a resin and 20 parts of rosin (rosiny thermal softening temperature 〉=85 ℃) and 2 parts of silicon-dioxide, make its dissolving postcooling to room temperature, the last isopropyl benzene hydroperoxide that adds 2 parts again stirs and is finished product.
Detect by the HB5315-85 standard:
Table one: be to add 20 weight part rosin and the intensity contrast that does not contain the rosiny anaerobic glue, T in the table
bBe breakdown torque, T
pBe removal torque; Other performance comparison sees Table two.
Add 20 weight part rosin as can be seen from Table I and do not contain the rosiny anaerobic glue when room temperature, its breakdown torque and removal torque are more or less the same; When temperature reached 85 ℃ of rosiny thermal softening point temperature, the rosin in the anaerobic glue was softening, and this moment, breakdown torque reduced about 50% with removal torque than not containing rosiny.When temperature during at 100 ℃, bonding strength is very little, has reduced by 80% than not containing rosin.
Add behind the 20 weight part rosin setting time as can be seen from Table II to anaerobic glue, stability, medium-resistance influence 80 ℃ the time are less.
Embodiment six: present embodiment is got 0.06 part of oxalic acid by weight and is joined and begin in 80 parts of Triethylene glycol dimethacrylate monomers to stir, be warming up to 50 ℃ and make its dissolving, add the adjacent benzenesulfonimides of 1 part of pyrodin and 1.5 parts again and stir 30 minutes to molten entirely, and then add 40 parts of fumaric acid bisphenol a resin and 30 parts of rosin (rosiny thermal softening temperature 〉=85 ℃) and 2 parts of silicon-dioxide, make its dissolving postcooling to room temperature, the isopropyl benzene hydroperoxide that adds 4 parts at last again stirred 30 minutes.
Detect by the HB5315-85 standard:
Table three: be to add 30 weight part rosin and the intensity contrast of not adding the rosiny anaerobic glue under differing temps, other performance comparison sees Table four.
As can be seen from Table III, add 30 weight part rosin and do not add the rosiny anaerobic glue under differing temps, its breakdown torque and removal torque are more or less the same; When temperature reached 85 ℃ of rosiny thermal softening point temperature, the rosin in the anaerobic glue was softening, and this moment, breakdown torque reduced about 60% with removal torque than not containing rosiny.
The rosin that adds 30 parts as can be seen from Table IV is little to other performance impact of anaerobic glue.
Embodiment seven: present embodiment is got 1 part of oxalic acid by weight and is joined and begin in 90 parts of Triethylene glycol dimethacrylate monomers to stir, be warming up to 55 ℃ and make its dissolving, add the adjacent benzenesulfonimides of 1.5 parts of pyrodins and 2.5 parts again and stir 30 minutes to molten entirely, and then add 30 parts of fumaric acid bisphenol a resin and 20 parts of nylon powders and 4 parts of silicon-dioxide, make its dissolving postcooling to room temperature, the isopropyl benzene hydroperoxide that adds 8 parts at last again stirred 30 minutes.
Detect by the HB5315-85 standard:
Table five: be to add 20 weight part nylon powders and the intensity contrast of not adding the anaerobic glue of nylon powder under differing temps, other performance comparison sees Table six.
As can be seen from Table V, add nylon powder and the anaerobic glue that does not add nylon powder under differing temps, its breakdown torque and removal torque are more or less the same; When temperature reached 150 ℃ of the thermal softening points of nylon powder, the nylon powder in the anaerobic glue was softening, this moment breakdown torque with removal torque than the reduction about 70% that does not contain nylon powder.
It is less to setting time of anaerobic glue, performance impact such as stability, media-resistant 80 ℃ the time to add 20 parts of nylon powders as can be seen from Table VI.
Table one: intensity contrast
Table two: other performance comparison
Table three: intensity contrast
Table four: other performance comparison
Table five: intensity contrast
Table six: other performance comparison
Claims (10)
1. low temperature detachable anaerobic adhesive is characterized in that it is made for 1～10 part by 50～95 parts of methacrylic acid diester monomers, 10～50 parts of unsaturated polyesters, 0.1～5 part of promotor, 0.1～5 part of adjacent benzenesulfonimide, 0.01～2 part of stablizer, 5～50 parts of thermal softening properties-correcting agent, 0.1～5 part of aerosil and organo-peroxide by weight.
2. a kind of low temperature detachable anaerobic adhesive according to claim 1 is characterized in that methacrylic acid diester monomer selects multicondensed ethylene glycol double methyl methacrylate, ethoxyquin dihydroxyphenyl propane dimethyl allene acid diester for use.
3. a kind of low temperature detachable anaerobic adhesive according to claim 1 is characterized in that unsaturated polyester selects the fumaric acid bisphenol a resin for use.
4. a kind of low temperature detachable anaerobic adhesive according to claim 1 is characterized in that promotor selects pyrodin, benzoyl hydrazine, N for use, N-dimethyl-p-toluidine, N, N-Diethyl Aniline or triethylamine.
5. a kind of low temperature detachable anaerobic adhesive according to claim 1 is characterized in that stablizer selects oxalic acid, ethylenediamine tetraacetic acid (EDTA), o-aminophenol, oxine, many pyridine compounds, phosphoric acid derivatives for use or select dihydroxy-benzene, benzoquinones, naphthoquinones, anthraquinone stopper for use.
6. a kind of low temperature detachable anaerobic adhesive according to claim 1 is characterized in that thermal softening properties-correcting agent selects rosin, maleated rosin, polymerized rosin, terpenes, rosin ester, nylon powder, polyethylene powders, polypropylene powder or polyvinyl chloride powder for use.
7. according to claim 1,2,3,4,5 or 6 described a kind of low temperature detachable anaerobic adhesives, it is characterized in that it is made for 1～5 part by 50～70 parts of methacrylic acid diester monomers, 10～30 parts of unsaturated polyesters, 0.1～2.5 part of promotor, 0.1～2.5 part of adjacent benzenesulfonimide, 0.01～1 part of stablizer, 5～25 parts of thermal softening properties-correcting agent, 0.1～2.5 part of aerosil and organo-peroxide by weight.
8. according to claim 1,2,3,4,5 or 6 described a kind of low temperature detachable anaerobic adhesives, it is characterized in that it is made for 6～10 parts by 71～90 parts of methacrylic acid diester monomers, 31～50 parts of unsaturated polyesters, 2.6～5 parts of promotor, 2.6～5 parts of adjacent benzenesulfonimides, 1.1～2 parts of stablizers, 26～50 parts of thermal softening properties-correcting agent, 2.6～5 parts of aerosils and organo-peroxide by weight.
9. a kind of low temperature detachable anaerobic adhesive according to claim 6 is characterized in that thermal softening temperature 〉=150 ℃ that thermal softening properties-correcting agent adopts rosiny thermal softening temperature 〉=85 ℃, adopts nylon powder.
10. the preparation method of a low temperature detachable anaerobic adhesive is characterized in that the preparation method is realized by the following step:
A, get 0.01～2 part of 50～95 parts of methacrylic acid diester monomer, stablizer earlier by weight and mix stirring, dissolving, stirred 30～120 minutes at 45～55 ℃;
B, in steps A, add promotor 0.1～5 weight part and adjacent benzenesulfonimide 0.1～5 weight part is stirred to molten entirely;
C, in step B, add unsaturated polyester 10～50 weight parts, thermal softening properties-correcting agent 5～50 weight parts and aerosil 0.1～5 weight part again, after treating to dissolve fully, be cooled to room temperature;
D, in step C, add organo-peroxide 1～10 weight part again and stir, promptly be prepared into low temperature detachable anaerobic adhesive.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338173B (en) * | 2007-07-04 | 2012-01-11 | 湖北回天胶业股份有限公司 | Single-component anaerobic structure glue and method for preparing same |
| CN101760141B (en) * | 2008-12-24 | 2012-02-08 | 湖北回天胶业股份有限公司 | High-temperature resistant high-storage stability flat sealing anaerbic adhesive and preparation method thereof |
| CN101497769B (en) * | 2009-02-23 | 2010-11-24 | 黑龙江省科学院石油化学研究院 | Inorganic / organic hybridized high temperature resistant anaerobic type screw thread locking sealing adhesive and preparation thereof |
| CN102876264A (en) * | 2012-09-25 | 2013-01-16 | 苏州汾湖电梯有限公司 | Anaerobic adhesive with high breakaway torque |
| CN104152086B (en) * | 2014-08-08 | 2017-01-18 | 黑龙江省科学院石油化学研究院 | Modified acrylate high temperature-resistant anaerobic adhesive and preparation method thereof |
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| JPS6210179A (en) * | 1985-07-09 | 1987-01-19 | Nippon Shokubai Kagaku Kogyo Co Ltd | Anaerobic adhesive composition |
| CN1159471A (en) * | 1996-11-15 | 1997-09-17 | 北京市天山新材料技术公司 | Anaerobic glue and preparation method |
| CN1226589A (en) * | 1998-02-19 | 1999-08-25 | 梁义勋 | Preparation of mono-component anaerobic adhesive for fastening screws and sealing flat surfaces |
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2005
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Patent Citations (3)
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|---|---|---|---|---|
| JPS6210179A (en) * | 1985-07-09 | 1987-01-19 | Nippon Shokubai Kagaku Kogyo Co Ltd | Anaerobic adhesive composition |
| CN1159471A (en) * | 1996-11-15 | 1997-09-17 | 北京市天山新材料技术公司 | Anaerobic glue and preparation method |
| CN1226589A (en) * | 1998-02-19 | 1999-08-25 | 梁义勋 | Preparation of mono-component anaerobic adhesive for fastening screws and sealing flat surfaces |
Non-Patent Citations (3)
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