CN109825242B - Anaerobic structural adhesive and preparation method thereof - Google Patents
Anaerobic structural adhesive and preparation method thereof Download PDFInfo
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- CN109825242B CN109825242B CN201910150661.5A CN201910150661A CN109825242B CN 109825242 B CN109825242 B CN 109825242B CN 201910150661 A CN201910150661 A CN 201910150661A CN 109825242 B CN109825242 B CN 109825242B
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Abstract
The invention discloses an anaerobic structural adhesive and a preparation method thereof, wherein the formula comprises the following components in parts by mass: 30-60 parts of urethane acrylate, 30-40 parts of acrylate monomer, 2-5 parts of accelerator, 3-5 parts of cross-linking agent, 1-5 parts of initiator, 0.5-1 part of stabilizer, 0.1-0.5 part of metal chelating agent and 0.5-1 part of dye; the anaerobic structural adhesive is suitable for fixing the magnetic steel of the motor, the selection of the formula accelerates the curing time of the structural adhesive, and enhances the bonding strength and impact resistance of the structural adhesive, so as to meet the use requirements of strong vibration, assembly line operation and high durability in the motor industry.
Description
Technical Field
The invention relates to the field of industrial material science, in particular to anaerobic structural adhesive for fixing motor magnetic steel and a preparation method thereof.
Background
With the development of society, the neodymium iron boron permanent magnet is most widely applied to motor products at present because the comprehensive performance of the neodymium iron boron permanent magnet is further improved. In the manufacturing process of motor products, because the motor products rotate at high speed and high frequency for a long time, how to firmly fix the magnetic steel (prevent the magnetic steel from falling off) is a major topic, and the reliability of the magnetic steel fixation becomes a key technology of the whole motor, and the quality reliability and the service life of the whole electromechanical equipment are directly influenced.
The adhesive for fixing the magnetic steel is always the focus of attention of technical personnel, and the currently applied adhesive usually comprises second-generation acrylate adhesive and modified epoxy adhesive, both of which have markets and have advantages and disadvantages. However, both of them have the problems of double components (low efficiency), big smell and toxicity, and are seriously not in accordance with the important issues of environmental protection and energy saving in China at present, so that the development of a single-component, high-efficiency and environment-friendly high-performance adhesive suitable for holding the motor magnetic steel is a problem to be solved urgently.
The anaerobic adhesive is an adhesive which has the function of inhibiting curing by utilizing acrylate monomers in the presence of oxygen and is cured automatically in an air-isolated manner, and has the characteristics of single component, oxygen-deficient fast curing at room temperature, no solvent, durability, drug resistance, low toxicity, aerobic storage for more than two years and the like. Has become an indispensable adhesive on assembly lines of electrical machinery automobile and airplane industry and the like, and has become an industrial adhesive which is difficult to replace by other adhesives in military industry such as aviation, aerospace, missile, cannonball and the like and mechanical product production departments of automobile, industrial machinery, petrochemical industry and various light and heavy industries. However, the traditional anaerobic adhesive is mainly applied to thread locking and sealing, and has the defects of slow curing, insufficient toughness and low bonding strength when applied to the magnetic steel fixing of the plane structure bonding, so that the use requirements of severe environments with strong vibration, high temperature and high humidity in the motor industry are difficult to meet; the present invention addresses these problems.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide the anaerobic structural adhesive and the preparation method thereof, the anaerobic structural adhesive is suitable for fixing the magnetic steel of the motor, the curing time of the structural adhesive is shortened, and the bonding strength and the impact resistance of the structural adhesive are enhanced, so that the use requirements of strong vibration, assembly line operation and high durability in the motor industry are met.
In order to achieve the above object, the present invention adopts the following technical solutions:
an anaerobic structural adhesive comprises the following components in parts by weight: 30-60 parts of urethane acrylate, 30-40 parts of acrylate monomer, 2-5 parts of accelerator, 3-5 parts of cross-linking agent, 1-5 parts of initiator, 0.5-1 part of stabilizer, 0.1-0.5 part of metal chelating agent and 0.5-1 part of dye.
The anaerobic structural adhesive comprises the following polyurethane acrylate: one or a mixture of more of bifunctional polyurethane acrylate, trifunctional polyurethane acrylate and polyfunctional polyurethane acrylate.
The anaerobic structural adhesive comprises the following acrylate monomers: isobornyl methacrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, methyl tetrahydrofuran acrylate, triethylene glycol dimethacrylate, polyethylene glycol dimethacrylate, trimethylolpropane triacrylate or a mixture of more than one of the above components.
The anaerobic structural adhesive comprises the following accelerators: one or a mixture of more of o-benzenesulfonimide, acetyl phenylhydrazine, ascorbic acid, triethylamine, N, N-dimethylaniline and tri-N-butylamine.
The anaerobic structural adhesive comprises the following cross-linking agents: one or more of methacrylic acid, acrylic acid and maleic acid.
The anaerobic structural adhesive comprises the following initiator: tert-butyl hydroperoxide, cumene hydroperoxide and dicumyl peroxide or a mixture of more of the tert-butyl hydroperoxide, the cumene hydroperoxide and the dicumyl peroxide.
The anaerobic structural adhesive comprises the following stabilizing agents: one or a mixture of several of p-tert-butylphenol, hydroquinone, p-benzoquinone and p-hydroxyanisole.
The anaerobic structural adhesive comprises a metal chelating agent and a water-soluble organic solvent, wherein the metal chelating agent comprises: one or more of ethylene diamine tetraacetic acid tetrasodium salt and ethylene diamine tetraacetic acid disodium salt.
The anaerobic structural adhesive comprises the following components in parts by weight: 20 parts of difunctional urethane acrylate, 40 parts of trifunctional urethane acrylate, 30 parts of hydroxypropyl methacrylate, 2 parts of acetyl phenylhydrazine, 3 parts of methacrylic acid, 5 parts of tert-butyl hydroperoxide, 1 part of hydroquinone, 0.3 part of ethylene diamine tetraacetic acid tetrasodium salt and 1 part of oil green.
The preparation method of the anaerobic structural adhesive comprises the following steps:
preparing materials according to a formula; the formula comprises the following components in parts by mass: 30-60 parts of urethane acrylate, 30-40 parts of acrylate monomer, 2-5 parts of accelerator, 3-5 parts of cross-linking agent, 1-5 parts of initiator, 0.5-1 part of stabilizer, 0.1-0.5 part of metal chelating agent and 0.5-1 part of dye;
putting urethane acrylate, an acrylate monomer, an accelerator, a cross-linking agent, an initiator, a stabilizer and a pigment into a reaction kettle according to parts by weight, fully stirring at 50-60 ℃ until the substances are completely dissolved, cooling to below 45 ℃, adding the initiator into the reaction kettle, uniformly stirring, filtering and discharging to obtain a finished product.
The invention has the advantages that:
according to the invention, by adding the low-functionality and high-functionality polyurethane acrylate prepolymer and the monomer, the high flexibility and high adhesive force of the low-functionality polyurethane acrylate, the fast curing and high glass transition temperature of the high-functionality polyurethane acrylate, the dilutability and the adhesive property of the monomer are utilized, and the adhesive strength and the impact resistance of the structural adhesive are enhanced;
then the curing time of the structural adhesive is accelerated by matching with the crosslinking density of the crosslinking agent;
the structural adhesive meets the use requirements of strong vibration, assembly line operation and high durability in the motor industry.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
An anaerobic structural adhesive comprises the following components in parts by weight: 30-60 parts of urethane acrylate, 30-40 parts of acrylate monomer, 2-5 parts of accelerator, 3-5 parts of cross-linking agent, 1-5 parts of initiator, 0.5-1 part of stabilizer, 0.1-0.5 part of metal chelating agent and 0.5-1 part of dye.
The urethane acrylate includes: one or a mixture of more of bifunctional polyurethane acrylate, trifunctional polyurethane acrylate and polyfunctional polyurethane acrylate.
The acrylate monomers include: isobornyl methacrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, methyl tetrahydrofuran acrylate, triethylene glycol dimethacrylate, polyethylene glycol dimethacrylate, trimethylolpropane triacrylate
The accelerator comprises: one or a mixture of more of o-benzenesulfonimide, acetyl phenylhydrazine, ascorbic acid, triethylamine, N, N-dimethylaniline and tri-N-butylamine.
The crosslinking agent comprises: one or more of methacrylic acid, acrylic acid and maleic acid.
The initiator comprises: tert-butyl hydroperoxide, cumene hydroperoxide and dicumyl peroxide or a mixture of more of the tert-butyl hydroperoxide, the cumene hydroperoxide and the dicumyl peroxide.
The stabilizer comprises: one or a mixture of several of p-tert-butylphenol, hydroquinone, p-benzoquinone and p-hydroxyanisole.
The metal chelating agent includes: one or more of ethylene diamine tetraacetic acid tetrasodium salt and ethylene diamine tetraacetic acid disodium salt.
The preparation method of the anaerobic structural adhesive comprises the following steps:
preparing materials according to a formula;
putting urethane acrylate, an acrylate monomer, an accelerator, a cross-linking agent, an initiator, a stabilizer and a pigment into a reaction kettle according to parts by weight, fully stirring at 50-60 ℃ until the substances are completely dissolved, cooling to below 45 ℃, adding the initiator into the reaction kettle, uniformly stirring, filtering and discharging to obtain a finished product.
Experiment one: the formula of the invention has the effects of enhancing the bonding strength and impact resistance of the structural adhesive and short curing time;
example 1:
a high-strength fast-curing anaerobic structural adhesive for fixing motor magnetic steel comprises the following components:
20g of difunctional urethane acrylate, 40g of trifunctional urethane acrylate, 30g of hydroxypropyl methacrylate, 2g of acetyl phenylhydrazine, 3g of methacrylic acid, 5g of tert-butyl hydroperoxide, 1g of hydroquinone, 0.3g of ethylene diamine tetraacetic acid tetrasodium salt and 1g of oil green;
example 2:
a high-strength fast-curing anaerobic structural adhesive for fixing motor magnetic steel comprises the following components:
25g of difunctional urethane acrylate, 30g of tetrafunctional urethane acrylate, 25g of hydroxypropyl methacrylate, 15g of isobornyl methacrylate, 2.5g of o-phenylsulfonyl imide, 5g of maleic acid, 3g of cumene hydroperoxide, 0.7g of hydroquinone, 0.1g of ethylenediaminetetraacetic acid tetrasodium salt and 0.8g of oil-containing blue;
example 3:
a high-strength fast-curing anaerobic structural adhesive for fixing motor magnetic steel comprises the following components:
20g of difunctional urethane acrylate, 10g of tetrafunctional urethane acrylate, 25g of methyl tetrahydrofuran acrylate, 15g of hydroxyethyl methacrylate, 3g of o-phenylsulfonyl imide, 2g of N, N-dimethylaniline, 4g of acrylic acid, 1g of dicumyl peroxide, 0.5g of p-hydroxyanisole, 0.5g of disodium ethylenediamine tetraacetate and 0.5g of oil-containing red;
comparative example 1:
a conventional anaerobic adhesive comprises the following components:
75g of epoxy methacrylate, 25g of hydroxyethyl methacrylate, 0.2g of hydroquinone, 0.05g of ethylene diamine tetraacetic acid tetrasodium salt, 2g of triethylamine and 5g of cumene hydroperoxide;
when the paint is prepared, the polyurethane acrylate, the acrylate monomer, the accelerator, the cross-linking agent, the initiator, the stabilizer and the pigment are put into a reaction kettle according to the components, fully stirred at 50-60 ℃ until the components are completely dissolved, cooled to below 45 ℃, added into the reaction kettle, uniformly stirred, filtered and discharged to obtain finished products 1, 2 and 3 and a comparative finished product 1.
And (3) testing positioning time: the test is carried out according to ASTM 5363-1997 standard, and carbon steel M10 bolts and nuts after being degreased by acetone are used as test objects, and the time period from the completion of assembly to the time of being screwed by hands without movement is carried out after sizing.
Tensile shear strength: according to the GB/T7124-2008 standard, the tensile shear strength of the adhesive (rigid material to rigid material) is measured by an electronic tensile machine. Two carbon steel sheets are cleaned by solvent and then ground by sand paper, the area of about 25 multiplied by 12.5mm is coated with glue, the two sheets are tightly adhered, a clamp is clamped tightly, and the carbon steel sheets are placed for more than 24 hours for tensile test.
Impact strength: according to the pendulum impact tester specified in GB/T6328-1999 standard.
The results of the test experiments on the finished products obtained in the examples and comparative examples are as follows:
as can be seen from the above table, compared with the comparative example, the high-strength fast-curing anaerobic structural adhesive for holding the motor magnetic steel prepared by the invention has the advantages that the bonding strength (shear strength) is greatly improved, the impact strength is obviously improved, the positioning time is more prominent, and the fast curing can be realized even in the low-temperature environment in winter. In addition, the structural adhesive is excellent in temperature resistance, and has high bonding strength even at 150 ℃; the formula of the invention has the effects of enhancing the bonding strength and impact resistance of the structural adhesive and shortening the curing time.
Experiment two: the combination of the urethane acrylate and the acrylate monomer is verified to enhance the bonding strength and the impact resistance of the structural adhesive;
example 4:
the components are as follows:
20g of difunctional urethane acrylate, 40g of trifunctional urethane acrylate, 2g of acetyl phenylhydrazine, 3g of methacrylic acid, 5g of tert-butyl hydroperoxide, 1g of hydroquinone, 0.3g of ethylenediaminetetraacetic acid tetrasodium salt and 1g of oil green;
this example lacks the acrylate monomer compared to example 1;
in the case of the example 5, the following examples were conducted,
the components are as follows:
30g of hydroxypropyl methacrylate, 2g of acetyl phenylhydrazine, 3g of methacrylic acid, 5g of tert-butyl hydroperoxide, 1g of hydroquinone, 0.3g of ethylene diamine tetraacetic acid tetrasodium salt and 1g of oil green;
this example lacks urethane acrylate compared to example 1;
during preparation, the components except the initiator are put into a reaction kettle according to the components, fully stirred at 50-60 ℃ until the components are completely dissolved, cooled to below 45 ℃, added into the reaction kettle, uniformly stirred, filtered and discharged, and the finished products 4 and 5 are obtained.
And (3) testing positioning time: the test is carried out according to ASTM 5363-1997 standard, and carbon steel M10 bolts and nuts after being degreased by acetone are used as test objects, and the time period from the completion of assembly to the time of being screwed by hands without movement is carried out after sizing.
Tensile shear strength: according to the GB/T7124-2008 standard, the tensile shear strength of the adhesive (rigid material to rigid material) is measured by an electronic tensile machine. Two carbon steel sheets are cleaned by solvent and then ground by sand paper, the area of about 25 multiplied by 12.5mm is coated with glue, the two sheets are tightly adhered, a clamp is clamped tightly, and the carbon steel sheets are placed for more than 24 hours for tensile test.
Impact strength: tested according to GB/T6328-1999 standard.
The results of the test experiments on the finished product obtained in the examples are as follows:
and (4) analyzing results: from the results of the second experiment, it is known that the combination of urethane acrylate and acrylate monomer can enhance the adhesive strength and impact resistance of the structural adhesive.
Experiment III, the selection of the accelerator is verified to shorten the curing time;
example 6:
the components are as follows:
20g of difunctional urethane acrylate, 40g of trifunctional urethane acrylate, 30g of hydroxypropyl methacrylate, 2g of o-phenylsulfonylimide, 3g of methacrylic acid, 5g of tert-butyl hydroperoxide, 1g of hydroquinone, 0.3g of ethylenediaminetetraacetic acid tetrasodium salt and 1g of oil green;
example 6 is different from example 1 in that the components of the accelerator are selected differently and the amounts are the same;
example 7
The components are as follows:
20g of difunctional urethane acrylate, 40g of trifunctional urethane acrylate, 30g of hydroxypropyl methacrylate, 6g of acetyl phenylhydrazine, 3g of methacrylic acid, 5g of tert-butyl hydroperoxide, 1g of hydroquinone, 0.3g of ethylene diamine tetraacetic acid tetrasodium salt and 1g of oil green;
example 7 differs from example 1 in that the accelerator components are selected identically and in different amounts.
During preparation, the components except the initiator are put into a reaction kettle according to the components, fully stirred at 50-60 ℃ until the components are completely dissolved, cooled to below 45 ℃, added into the reaction kettle, uniformly stirred, filtered and discharged, and the finished products 6 and 7 are obtained.
And (3) testing positioning time: the test is carried out according to ASTM 5363-1997 standard, and carbon steel M10 bolts and nuts after being degreased by acetone are used as test objects, and the time period from the completion of assembly to the time of being screwed by hands without movement is carried out after sizing.
Tensile shear strength: according to the GB/T7124-2008 standard, the tensile shear strength of the adhesive (rigid material to rigid material) is measured by an electronic tensile machine. Two carbon steel sheets are cleaned by solvent and then ground by sand paper, the area of about 25 multiplied by 12.5mm is coated with glue, the two sheets are tightly adhered, a clamp is clamped tightly, and the carbon steel sheets are placed for more than 24 hours for tensile test.
Impact strength: tested according to GB/T6328-1999 standard.
The results of the test experiments on the finished product obtained in the examples are as follows:
and (4) analyzing results: from the results of experiment three, it is clear that the selection of the accelerator can reduce the curing time. However, when selecting acetophenone hydrazine as an accelerator, the improvement of the curing time is not obvious in 2 parts and 6 parts, and the storage stability is also considered in practical application, so 2 parts is selected as the optimum.
The optimal formula is comprehensively judged by the three experiments and comprises the following components in parts by weight: 20 parts of difunctional urethane acrylate, 40 parts of trifunctional urethane acrylate, 30 parts of hydroxypropyl methacrylate, 2 parts of acetyl phenylhydrazine, 3 parts of methacrylic acid, 5 parts of tert-butyl hydroperoxide, 1 part of hydroquinone, 0.3 part of ethylene diamine tetraacetic acid tetrasodium salt and 1 part of oil green.
According to the invention, by adding the low-functionality and high-functionality polyurethane acrylate prepolymer and the monomer, the high flexibility and high adhesive force of the low-functionality polyurethane acrylate, the fast curing and high glass transition temperature of the high-functionality polyurethane acrylate, the dilutability and the adhesive property of the monomer are utilized, and the adhesive strength and the impact resistance of the structural adhesive are enhanced; then the curing time of the structural adhesive is accelerated by matching with the crosslinking density of the crosslinking agent; the structural adhesive meets the use requirements of strong vibration, assembly line operation and high durability in the motor industry.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It should be understood by those skilled in the art that the above embodiments do not limit the present invention in any way, and all technical solutions obtained by using equivalent alternatives or equivalent variations fall within the scope of the present invention.
Claims (2)
1. The anaerobic structural adhesive is characterized by comprising the following components in parts by weight: 20 parts of difunctional urethane acrylate, 40 parts of trifunctional urethane acrylate, 30 parts of hydroxypropyl methacrylate, 2 parts of acetyl phenylhydrazine, 3 parts of methacrylic acid, 5 parts of tert-butyl hydroperoxide, 1 part of hydroquinone, 0.3 part of ethylene diamine tetraacetic acid tetrasodium salt and 1 part of oil green.
2. The preparation method of the anaerobic structural adhesive is characterized by comprising the following steps:
preparing materials according to a formula; the formula comprises the following components in parts by mass: 20 parts of difunctional urethane acrylate, 40 parts of trifunctional urethane acrylate, 30 parts of hydroxypropyl methacrylate, 2 parts of acetyl phenylhydrazine, 3 parts of methacrylic acid, 5 parts of tert-butyl hydroperoxide, 1 part of hydroquinone, 0.3 part of ethylene diamine tetraacetic acid tetrasodium salt and 1 part of oil green;
putting the raw materials except the tert-butyl hydroperoxide into a reaction kettle according to the mass portion, fully stirring the raw materials at 50-60 ℃ until the raw materials are completely dissolved, cooling the mixture to below 45 ℃, adding the tert-butyl hydroperoxide into the reaction kettle, uniformly stirring the mixture, filtering and discharging the mixture to obtain a finished product.
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| CN112126386A (en) * | 2020-09-24 | 2020-12-25 | 邵阳把兄弟新材料科技有限公司 | Low-temperature-resistant refrigerating pipeline sealant and preparation method and application thereof |
| CN112341981A (en) * | 2020-10-27 | 2021-02-09 | 深圳市帕克威乐新材料有限公司 | Anaerobic adhesive and preparation method thereof |
| CN113999644A (en) * | 2021-11-24 | 2022-02-01 | 浙江科力厌氧胶有限公司 | UV adhesive and preparation method thereof |
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| WO2013079952A1 (en) * | 2011-12-01 | 2013-06-06 | Spinnaker International Limited | Adhesive composition |
| CN103342966A (en) * | 2013-07-02 | 2013-10-09 | 广东恒大新材料科技有限公司 | High-strength high-temperature-resistant structural anaerobic adhesive and preparation method thereof |
| CN107722842A (en) * | 2017-11-07 | 2018-02-23 | 广东三和控股有限公司 | A kind of quick-drying, high stability anaerobic adhesive and preparation method thereof |
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| WO2013079952A1 (en) * | 2011-12-01 | 2013-06-06 | Spinnaker International Limited | Adhesive composition |
| CN103342966A (en) * | 2013-07-02 | 2013-10-09 | 广东恒大新材料科技有限公司 | High-strength high-temperature-resistant structural anaerobic adhesive and preparation method thereof |
| CN107722842A (en) * | 2017-11-07 | 2018-02-23 | 广东三和控股有限公司 | A kind of quick-drying, high stability anaerobic adhesive and preparation method thereof |
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| 高强度厌氧结构胶的研制及其影响因素研究;曹芳维等;《中国胶粘剂》;20161130;第25卷(第11期);第34-36页 * |
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