CN106675498A - Anaerobic adhesive and preparation method thereof - Google Patents
Anaerobic adhesive and preparation method thereof Download PDFInfo
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- CN106675498A CN106675498A CN201611044370.0A CN201611044370A CN106675498A CN 106675498 A CN106675498 A CN 106675498A CN 201611044370 A CN201611044370 A CN 201611044370A CN 106675498 A CN106675498 A CN 106675498A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
- C09J163/10—Epoxy resins modified by unsaturated compounds
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Abstract
The invention discloses an anaerobic adhesive and a preparation method thereof. The anaerobic adhesive is composed of the following raw materials in parts by weight: 20-25 parts of hydroxyethyl methylacrylate, 8-15 parts of polyurethane acrylate, 8-12 parts of epoxy acrylate, 40-45 parts of precipitated silicon dioxide, 4-5 parts of a thixotropic agent, 1-2 parts of hydroxyethyl acrylate, 1-1.5 parts of trimethylolpropane triacrylate, 0.1-0.3 part of acrylic acid, 1-3 parts of isopropyl benzene hydroperoxide, 1-3 parts of N,N-dimethylaniline, 0.3-0.8 part of o-benzoic sulfimide, 0.5-1 part of a polymerization inhibitor, 0.1-0.5 part of a coupling agent and 0.01-0.05 part of disodium ethylene diamine tetraacetate. The anaerobic adhesive disclosed by the invention has the characteristics of being low in cost of raw materials, high in strength, high in hardness, high in viscosity and good in storage stability.
Description
Technical field
The present invention relates to be applied to industrial bonding agent field.It is more particularly related to a kind of anaerobic adhesive and
Its preparation method.
Background technology
In recent years, the development of anaerobic adhesive is more and more faster, and market competition is also increasing, in this case, studies a
Superior performance, cheap, environment-friendly anaerobic adhesive are necessary.Precipitated silicon dioxide is used as conventional filling material
Material, have environment-protecting asepsis, it is cheap, enhancing reinforcement the features such as, be used as the filler of anaerobic adhesive, can with reduces cost,
Improve hardness, increase intensity, but simultaneously as precipitated silica is with the extension of standing time, easily deposition, and produce point
Layer phenomenon, causes the storage time of anaerobic adhesive short.
The content of the invention
It is an object of the invention to solve at least the above, and provide the advantage that at least will be described later.
High viscosity thixotroping anaerobic adhesive it is a still further object of the present invention to provide a kind of stable storing and preparation method thereof.
In order to realize these purposes of the invention and further advantage, there is provided a kind of anaerobic adhesive, by part by weight
The following raw material composition：Hydroxyethyl methacrylate 20-25 parts, urethane acrylate 8-15 parts, epoxy acrylate 8-12
Part, precipitated silica 40-45 parts, thixotropic agent 4-5 parts, hydroxy-ethyl acrylate 1-2 parts, trimethylolpropane trimethacrylate 1-
1.5 parts, acrylic acid 0.1-0.3 parts, isopropyl benzene hydroperoxide 1-3 parts, N, accelerine 1-3 parts, o-benzoyl sulphonyl Asia
Amine 0.3-0.8 parts, polymerization inhibitor 0.5-1 parts, coupling agent 0.1-0.5 parts and disodium ethylene diamine tetraacetate 0.01-0.05 parts.
Preferably, thixotropic agent is made up of the following raw material of part by weight：60-65 parts of BYK-410 thixotropic agent, gas phase two
Silica 3-5 parts, organobentonite 1-3 parts, kaolin 4-5 parts and paraffin oil 20-25 parts.
Preferably, polymerization inhibitor is made up of the following raw material of part by weight：Hydroquinones 20-25 parts, 1,4-benzoquinone 10-15
Part, MEHQ 6-10 parts, petroleum ether 25-28 parts and glycerine 18-24 parts.
Preferably, coupling agent is made up of the following raw material of part by weight：Silane coupling agent KH550 40-45 parts, it is hard
Resin acid 10-20 parts, methylisobutylketone 15-20 parts, expoxy propane 5-10 parts.
The present invention also provides a kind of preparation method of anaerobic adhesive, comprises the following steps：
Step one, by the hydroxyethyl methacrylate of above-mentioned weight portion, urethane acrylate, epoxy acrylate, heavy
Shallow lake silica, thixotropic agent, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate, acrylic acid, isopropyl benzene hydroperoxide,
N, accelerine, o-benzoic sulfimide, polymerization inhibitor, coupling agent and disodium ethylene diamine tetraacetate are put into mixer
Uniform stirring 2-2.5 hours, then filter and mixed solution is obtained；
Step 2,20-30 minutes prepared anaerobic adhesive is kept by the mixed solution under 3-5KPa air pressure.
Preferably, in the step one, first by the hydroxyethyl methacrylate of above-mentioned weight portion, polymerization inhibitor, ethylenediamine
The acrylic acid of tetraacethyl disodium and above-mentioned weight portion heats 30 DEG C and places into stirring in mixer, treats that solid is completely dissolved, then add
Enter urethane acrylate, epoxy acrylate, precipitated silica, thixotropic agent, hydroxy-ethyl acrylate, three of above-mentioned weight portion
Hydroxymethyl-propane triacrylate, DMA, o-benzoic sulfimide, coupling agent are well mixed, and are eventually adding
Isopropyl benzene hydroperoxide.
Preferably, also included before step 2 after the step one：
Step a, the mixed solution is put into reactor, will take out low pressure to 0-10KPa in reactor, is warming up to 20-
25 DEG C, with the Ultrasonic Radiation of 33-35KHz in low pressure and temperature-rise period is taken out, then will recover normal pressure in reactor and be down to
Room temperature；
Step b, will take out low pressure to 15-20KPa in reactor, be warming up to 25-30 DEG C, be used in low pressure and temperature-rise period is taken out
The Ultrasonic Radiation of 30-32KHz, then will recover normal pressure and is down to room temperature in reactor；
Step c, will take out low pressure to 20-25KPa in reactor, be warming up to 30-35 DEG C, be used in low pressure and temperature-rise period is taken out
The Ultrasonic Radiation of 25-28KHz, then will recover normal pressure and be down to room temperature in reactor, and to addition 20-40 weights in reactor
Amount part deionized water.
The present invention at least includes following beneficial effect：
1st, the cost of material of anaerobic adhesive of the present invention is low.
2nd, anaerobic adhesive of the present invention has high intensity, high rigidity and high-viscosity feature.
3rd, the storage stability of anaerobic adhesive of the present invention is high, and storage for a long time does not occur layering failure phenomenon.
Further advantage of the invention, target and feature embody part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to specification
Word can be implemented according to this.
It should be noted that experimental technique described in following embodiments, unless otherwise specified, is conventional method, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained.
A kind of anaerobic adhesive, is made up of the following raw material of part by weight：Hydroxyethyl methacrylate 20-25 parts, polyurethane
Acrylate 8-15 parts, epoxy acrylate 8-12 parts, precipitated silica 40-45 parts, thixotropic agent 4-5 parts, acrylic acid hydroxyl second
Ester 1-2 parts, trimethylolpropane trimethacrylate 1-1.5 parts, acrylic acid 0.1-0.3 parts, isopropyl benzene hydroperoxide 1-3 parts, N,
Accelerine 1-3 parts, o-benzoic sulfimide 0.3-0.8 parts, polymerization inhibitor 0.5-1 parts, coupling agent 0.1-0.5 parts and
Disodium ethylene diamine tetraacetate 0.01-0.05 parts.
In the present invention, hydroxyethyl methacrylate rises as the material of main part of the anaerobic adhesive and ensures that anaerobism glue sticking is strong
The effect of degree；Urethane acrylate is also one of material of main part of anaerobic adhesive, acts the work for ensureing colloid mobility and adhesive force
With；The effect of epoxy acrylate is the glued membrane hardness for strengthening anaerobic adhesive；The effect of precipitated silica is that anaerobic adhesive is thickened
And hardening, reduce cost of material；The effect of thixotropic agent is when being arranged in pairs or groups using come the storage for extending anaerobic adhesive with precipitated silica
Between；The effect of hydroxy-ethyl acrylate is the solubility for increasing each component in anaerobic adhesive；Trimethylolpropane trimethacrylate
Effect is the colloid density for improving anaerobic adhesive；Acrylic acid effect is the adhesive strength for increasing anaerobic adhesive；Isopropyl benzene hydroperoxide
Effect be initiator, trigger anaerobic adhesive each component between reaction；The effect of DMA is accelerator, promotes to detest
Reaction between oxygen glue each component；The effect of o-benzoic sulfimide is kicker, and accelerator can be made to play most your writing
With reduction accelerator dosage；The effect of polymerization inhibitor is anaerobic adhesive each component is not crosslinked reaction using preceding, keeps anaerobic adhesive
Use preceding stability；The effect of coupling agent is the adhesive force for improving anaerobic adhesive；The effect of disodium ethylene diamine tetraacetate is metal
Complex in ion chelating agent, with anaerobic adhesive, prevents heavy metal ion from playing side effect.
Embodiment 1：
A kind of anaerobic adhesive, is made up of the following raw material of part by weight：20 parts of hydroxyethyl methacrylate, polyurethane propylene
8 parts of acid esters, 8 parts of epoxy acrylate, 40 parts of precipitated silica, 4 parts of thixotropic agent, 1 part of hydroxy-ethyl acrylate, trihydroxy methyl third
1 part of alkane triacrylate, 0.1 part of acrylic acid, 1 part of isopropyl benzene hydroperoxide, N, 1 part of accelerine, o-benzoyl sulphonyl
0.01 part of 0.3 part of imines, 0.5 part of polymerization inhibitor, 0.1 part of coupling agent and disodium ethylene diamine tetraacetate.
Thixotropic agent is BYK-410, and polymerization inhibitor is polymerization inhibitor 510, and coupling agent can be Silane coupling agent KH550 or carbonic acid
Calcium or alumina silicate one of which.
By the hydroxyethyl methacrylate of above-mentioned weight portion, urethane acrylate, epoxy acrylate, precipitated silica
Silicon, thixotropic agent, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate, acrylic acid, isopropyl benzene hydroperoxide, N, N- diformazans
Base aniline, o-benzoic sulfimide, polymerization inhibitor, coupling agent and disodium ethylene diamine tetraacetate are put into uniform stirring in mixer
2 hours, then filter and mixed solution is obtained, the mixed solution is kept into 20 minutes prepared anaerobic adhesives under 3KPa air pressure.
Embodiment 2：
A kind of anaerobic adhesive, is made up of the following raw material of part by weight：25 parts of hydroxyethyl methacrylate, polyurethane propylene
15 parts of acid esters, 12 parts of epoxy acrylate, 45 parts of precipitated silica, 5 parts of thixotropic agent, 2 parts of hydroxy-ethyl acrylate, trihydroxy methyl
1.5 parts of propane triacrylate, 0.3 part of acrylic acid, 3 parts of isopropyl benzene hydroperoxide, N, 3 parts of accelerine, o-benzoyl
0.05 part of 0.8 part of sulfimide, 1 part of polymerization inhibitor, 0.5 part of coupling agent and disodium ethylene diamine tetraacetate.
Thixotropic agent is BYK-410, and polymerization inhibitor is polymerization inhibitor 510, and coupling agent can be Silane coupling agent KH550 or carbonic acid
Calcium or alumina silicate one of which.
By the hydroxyethyl methacrylate of above-mentioned weight portion, urethane acrylate, epoxy acrylate, precipitated silica
Silicon, thixotropic agent, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate, acrylic acid, isopropyl benzene hydroperoxide, N, N- diformazans
Base aniline, o-benzoic sulfimide, polymerization inhibitor, coupling agent and disodium ethylene diamine tetraacetate are put into uniform stirring in mixer
2.5 hours, then filter and mixed solution is obtained, the mixed solution is kept into 30 minutes prepared anaerobic adhesives under 5KPa air pressure.
Embodiment 3：
A kind of anaerobic adhesive, is made up of the following raw material of part by weight：23 parts of hydroxyethyl methacrylate, polyurethane propylene
12 parts of acid esters, 10 parts of epoxy acrylate, 43 parts of precipitated silica, 4.5 parts of thixotropic agent, 1.5 parts of hydroxy-ethyl acrylate, three hydroxyls
1.25 parts of propane tri, 0.2 part of acrylic acid, 2 parts of isopropyl benzene hydroperoxide, N, 2 parts of accelerine, adjacent benzene
0.03 part of 0.5 part of formyl sulfimide, 0.7 part of polymerization inhibitor, 0.3 part of coupling agent and disodium ethylene diamine tetraacetate.
Thixotropic agent is BYK-410, and polymerization inhibitor is polymerization inhibitor 510, and coupling agent can be Silane coupling agent KH550 or carbonic acid
Calcium or alumina silicate one of which.
By the hydroxyethyl methacrylate of above-mentioned weight portion, urethane acrylate, epoxy acrylate, precipitated silica
Silicon, thixotropic agent, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate, acrylic acid, isopropyl benzene hydroperoxide, N, N- diformazans
Base aniline, o-benzoic sulfimide, polymerization inhibitor, coupling agent and disodium ethylene diamine tetraacetate are put into uniform stirring in mixer
2.3 hours, then filter and mixed solution is obtained, the mixed solution is kept into 25 minutes prepared anaerobic adhesives under 4KPa air pressure.
Comparative example 1：
A kind of anaerobic adhesive, is made up of the following raw material of part by weight：23 parts of hydroxyethyl methacrylate, polyurethane propylene
12 parts of acid esters, 10 parts of epoxy acrylate, 43 parts of precipitated silica, 1.5 parts of hydroxy-ethyl acrylate, trimethylolpropane tris third
1.25 parts of olefin(e) acid ester, 0.2 part of acrylic acid, 2 parts of isopropyl benzene hydroperoxide, N, 2 parts of accelerine, o-benzoic sulfimide
0.03 part of 0.5 part, 0.7 part of polymerization inhibitor, 0.3 part of coupling agent and disodium ethylene diamine tetraacetate.
Polymerization inhibitor is polymerization inhibitor 510, coupling agent can be Silane coupling agent KH550 or calcium carbonate or alumina silicate wherein
It is a kind of.
By the hydroxyethyl methacrylate of above-mentioned weight portion, urethane acrylate, epoxy acrylate, precipitated silica
Silicon, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate, acrylic acid, isopropyl benzene hydroperoxide, N, accelerine,
It is small that o-benzoic sulfimide, polymerization inhibitor, coupling agent and disodium ethylene diamine tetraacetate are put into uniform stirring 2.3 in mixer
When, then filter and mixed solution is obtained, the mixed solution is kept into 25 minutes prepared anaerobic adhesives under 4KPa air pressure.
Following table is the performance table of comparisons of the embodiment with comparative example of anaerobic adhesive of the present invention：
The storage stability of anaerobic adhesive is measured using the method for air standard HB5329-93 in table, and characterize data is
The viscosity build rate of anaerobic adhesive.
By data in contrast table, each component content of the anaerobic adhesive is：It is 23 parts of hydroxyethyl methacrylate, poly-
12 parts of urethane acrylate, 10 parts of epoxy acrylate, 43 parts of precipitated silica, 4.5 parts of thixotropic agent, hydroxy-ethyl acrylate
1.5 parts, 1.25 parts of trimethylolpropane trimethacrylate, 0.2 part of acrylic acid, 2 parts of isopropyl benzene hydroperoxide, N, N- dimethyl benzenes
0.03 part of 2 parts of amine, 0.5 part of o-benzoic sulfimide, 0.7 part of polymerization inhibitor, 0.3 part of coupling agent and disodium ethylene diamine tetraacetate
When, various aspects of performance is preferable, meanwhile, the storage stability of anaerobic adhesive is also improved after the appropriate thixotropic agent of addition, because touching
Become the network structure that agent forms three-dimensional in oleaginous system, easily so that the viscosity of anaerobic adhesive becomes very big and nothing in the present invention
Method is layered, and this structure only can just be destroyed when by mechanical forces, and viscosity declines, and liquid-phase system recovers good stream
Dynamic property.Unstable problem is stored invention not only improves what colloidal solution layering brought, anaerobism is not interfered with when using yet
The mobility of glue.
Embodiment 4：
A kind of anaerobic adhesive, is made up of the following raw material of part by weight：23 parts of hydroxyethyl methacrylate, polyurethane propylene
12 parts of acid esters, 10 parts of epoxy acrylate, 43 parts of precipitated silica, 4.5 parts of thixotropic agent, 1.5 parts of hydroxy-ethyl acrylate, three hydroxyls
1.25 parts of propane tri, 0.2 part of acrylic acid, 2 parts of isopropyl benzene hydroperoxide, N, 2 parts of accelerine, adjacent benzene
0.03 part of 0.5 part of formyl sulfimide, 0.7 part of polymerization inhibitor, 0.3 part of coupling agent and disodium ethylene diamine tetraacetate.
Thixotropic agent is made up of the following raw material of part by weight：60 parts of BYK-410 thixotropic agent, 3 parts of aerosil, have
20 parts of 1 part of machine bentonite, 4 parts of kaolin and paraffin oil.
Polymerization inhibitor is made up of the following raw material of part by weight：20 parts of hydroquinones, 10 parts of 1,4-benzoquinone, MEHQ
18 parts of 6 parts, 25 parts of petroleum ether and glycerine.
Coupling agent is made up of the following raw material of part by weight：40 parts of Silane coupling agent KH550,10 parts of stearic acid, methyl
15 parts of isobutyl ketone, 5 parts of expoxy propane.
First by the hydroxyethyl methacrylate of above-mentioned weight portion, polymerization inhibitor, disodium ethylene diamine tetraacetate and above-mentioned weight portion
Acrylic acid heat 30 DEG C and place into stirring in mixer, treat that solid is completely dissolved, add the polyurethane third of above-mentioned weight portion
Olefin(e) acid ester, epoxy acrylate, precipitated silica, thixotropic agent, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate,
DMA, o-benzoic sulfimide, coupling agent are well mixed, and are eventually adding isopropyl benzene hydroperoxide stirring 2.3
Hour, then filter and mixed solution is obtained.
The mixed solution is put into reactor, and takes out low pressure to 0KPa, be warming up to 20 DEG C, taken out low pressure and heating up
33KHz Ultrasonic Radiations are used in journey, then will be recovered normal pressure in reactor and be down to room temperature.
Low pressure to 15KPa will be taken out in reactor again, be warming up to 25 DEG C, with 30KHz ultrasounds in low pressure and temperature-rise period is taken out
Wave radiation, then will recover normal pressure and is down to room temperature in reactor,
Low pressure to 20KPa will be taken out in reactor again, be warming up to 30 DEG C, with 25KHz ultrasounds in low pressure and temperature-rise period is taken out
Wave radiation, then will recover normal pressure and to be down to room temperature in reactor, and to adding 20 parts by weight of deionized water in reactor.
25 minutes prepared anaerobic adhesives are kept under 4KPa air pressure to the solution obtained by previous step.
Embodiment 5：
A kind of anaerobic adhesive, is made up of the following raw material of part by weight：23 parts of hydroxyethyl methacrylate, polyurethane propylene
12 parts of acid esters, 10 parts of epoxy acrylate, 43 parts of precipitated silica, 4.5 parts of thixotropic agent, 1.5 parts of hydroxy-ethyl acrylate, three hydroxyls
1.25 parts of propane tri, 0.2 part of acrylic acid, 2 parts of isopropyl benzene hydroperoxide, N, 2 parts of accelerine, adjacent benzene
0.03 part of 0.5 part of formyl sulfimide, 0.7 part of polymerization inhibitor, 0.3 part of coupling agent and disodium ethylene diamine tetraacetate.
Thixotropic agent is made up of the following raw material of part by weight：65 parts of BYK-410 thixotropic agent, 5 parts of aerosil, have
25 parts of 3 parts of machine bentonite, 5 parts of kaolin and paraffin oil.
Polymerization inhibitor is made up of the following raw material of part by weight：25 parts of hydroquinones, 15 parts of 1,4-benzoquinone, MEHQ
24 parts of 10 parts, 28 parts of petroleum ether and glycerine.
Coupling agent is made up of the following raw material of part by weight：45 parts of Silane coupling agent KH550,20 parts of stearic acid, methyl
20 parts of isobutyl ketone, 10 parts of expoxy propane.
First by the hydroxyethyl methacrylate of above-mentioned weight portion, polymerization inhibitor, disodium ethylene diamine tetraacetate and above-mentioned weight portion
Acrylic acid heat 30 DEG C and place into stirring in mixer, treat that solid is completely dissolved, add the polyurethane third of above-mentioned weight portion
Olefin(e) acid ester, epoxy acrylate, precipitated silica, thixotropic agent, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate,
DMA, o-benzoic sulfimide, coupling agent are well mixed, and are eventually adding isopropyl benzene hydroperoxide stirring 2.3
Hour, then filter and mixed solution is obtained.
The mixed solution is put into reactor, and takes out low pressure to 10KPa, be warming up to 25 DEG C, taking out low pressure and intensification
During use 35KHz Ultrasonic Radiations, then will recover normal pressure and to be down to room temperature in reactor.
Low pressure to 20KPa will be taken out in reactor again, be warming up to 30 DEG C, with 32KHz ultrasounds in low pressure and temperature-rise period is taken out
Wave radiation, then will recover normal pressure and is down to room temperature in reactor,
Low pressure to 25KPa will be taken out in reactor again, be warming up to 35 DEG C, with 28KHz ultrasounds in low pressure and temperature-rise period is taken out
Wave radiation, then will recover normal pressure and to be down to room temperature in reactor, and to adding 40 parts by weight of deionized water in reactor.
25 minutes prepared anaerobic adhesives are kept under 4KPa air pressure to the solution obtained by previous step.
Embodiment 6：
A kind of anaerobic adhesive, is made up of the following raw material of part by weight：23 parts of hydroxyethyl methacrylate, polyurethane propylene
12 parts of acid esters, 10 parts of epoxy acrylate, 43 parts of precipitated silica, 4.5 parts of thixotropic agent, 1.5 parts of hydroxy-ethyl acrylate, three hydroxyls
1.25 parts of propane tri, 0.2 part of acrylic acid, 2 parts of isopropyl benzene hydroperoxide, N, 2 parts of accelerine, adjacent benzene
0.03 part of 0.5 part of formyl sulfimide, 0.7 part of polymerization inhibitor, 0.3 part of coupling agent and disodium ethylene diamine tetraacetate.
Thixotropic agent is made up of the following raw material of part by weight：65 parts of BYK-410 thixotropic agent, 5 parts of aerosil, have
25 parts of 3 parts of machine bentonite, 5 parts of kaolin and paraffin oil.
Polymerization inhibitor is made up of the following raw material of part by weight：25 parts of hydroquinones, 15 parts of 1,4-benzoquinone, MEHQ
24 parts of 10 parts, 28 parts of petroleum ether and glycerine.
Coupling agent is made up of the following raw material of part by weight：45 parts of Silane coupling agent KH550,20 parts of stearic acid, methyl
20 parts of isobutyl ketone, 10 parts of expoxy propane.
First by the hydroxyethyl methacrylate of above-mentioned weight portion, polymerization inhibitor, disodium ethylene diamine tetraacetate and above-mentioned weight portion
Acrylic acid heat 30 DEG C and place into stirring in mixer, treat that solid is completely dissolved, add the polyurethane third of above-mentioned weight portion
Olefin(e) acid ester, epoxy acrylate, precipitated silica, thixotropic agent, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate,
DMA, o-benzoic sulfimide, coupling agent are well mixed, and are eventually adding isopropyl benzene hydroperoxide stirring 2.3
Hour, then filter and mixed solution is obtained.
The mixed solution is put into reactor, and takes out low pressure to 5KPa, be warming up to 23 DEG C, taken out low pressure and heating up
34KHz Ultrasonic Radiations are used in journey, then will be recovered normal pressure in reactor and be down to room temperature.
Low pressure to 18KPa will be taken out in reactor again, be warming up to 28 DEG C, with 31KHz ultrasounds in low pressure and temperature-rise period is taken out
Wave radiation, then will recover normal pressure and is down to room temperature in reactor,
Low pressure to 23KPa will be taken out in reactor again, be warming up to 33 DEG C, with 26KHz ultrasounds in low pressure and temperature-rise period is taken out
Wave radiation, then will recover normal pressure and to be down to room temperature in reactor, and to adding 30 parts by weight of deionized water in reactor.
25 minutes prepared anaerobic adhesives are kept under 4KPa air pressure to the solution obtained by previous step.
Comparative example 2：
Embodiments thereof is same as Example 3.
Following table is the performance table of comparisons of the embodiment with comparative example of anaerobic adhesive of the present invention：
The storage stability of anaerobic adhesive is measured using the method for air standard HB5329-93 in table, and characterize data is
The viscosity build rate of anaerobic adhesive.
By data in contrast table, the best results of embodiment 6, and embodiment 4, embodiment 5 and embodiment 6 are relative
In comparative example 2, performance increases, because in a low voltage state, the oil components boiling point reduction in colloid, it is easy to
Vaporization, at the same the microbubble produced in the case of ultrasonic irradiation the shatter polymeric particles reunited together are on one side on one side
Vaporescence is accelerated, the droplet surface area after vaporization is easier to be well mixed greatly, and the defects such as segregation layering are not produced, it is ensured that
The various aspects of performance of colloid is more excellent.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in specification and implementation method
With, it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easily
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details.
Claims (7)
1. a kind of anaerobic adhesive, it is characterised in that be made up of the following raw material of part by weight：Hydroxyethyl methacrylate 20-25
Part, urethane acrylate 8-15 parts, epoxy acrylate 8-12 parts, precipitated silica 40-45 parts, thixotropic agent 4-5 parts, third
1-2 parts of olefin(e) acid hydroxyl ethyl ester, trimethylolpropane trimethacrylate 1-1.5 parts, acrylic acid 0.1-0.3 parts, isopropyl benzene hydroperoxide
1-3 parts, N, accelerine 1-3 parts, o-benzoic sulfimide 0.3-0.8 parts, polymerization inhibitor 0.5-1 parts, coupling agent 0.1-
0.5 part and disodium ethylene diamine tetraacetate 0.01-0.05 parts.
2. anaerobic adhesive as claimed in claim 1, it is characterised in that thixotropic agent is made up of the following raw material of part by weight：
60-65 parts, aerosil 3-5 parts, organobentonite 1-3 parts, kaolin 4-5 parts and paraffin oil 20- of BYK-410 thixotropic agent
25 parts.
3. anaerobic adhesive as claimed in claim 1, it is characterised in that polymerization inhibitor is made up of the following raw material of part by weight：It is right
Benzenediol 20-25 parts, 1,4-benzoquinone 10-15, MEHQ 6-10, petroleum ether 25-28 and glycerine 18-24.
4. anaerobic adhesive as claimed in claim 1, it is characterised in that coupling agent is made up of the following raw material of part by weight：Silicon
40-45 parts, stearic acid 10-20 parts, methylisobutylketone 15-20 parts, expoxy propane 5-10 parts of alkane coupling agent KH550.
5. a kind of preparation method of anaerobic adhesive as claimed in claim 1, it is characterised in that comprise the following steps：
Step one, by the hydroxyethyl methacrylate of above-mentioned weight portion, urethane acrylate, epoxy acrylate, precipitation two
Silica, thixotropic agent, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate, acrylic acid, isopropyl benzene hydroperoxide, N, N-
Dimethylaniline, o-benzoic sulfimide, polymerization inhibitor, coupling agent and disodium ethylene diamine tetraacetate are put into mixer uniformly
Stirring 2-2.5 hours, then filters and mixed solution is obtained；
Step 2,20-30 minutes prepared anaerobic adhesive is kept by the mixed solution under 3-5KPa air pressure.
6. preparation method as claimed in claim 5, it is characterised in that in the step one, first by the methyl of above-mentioned weight portion
The acrylic acid of hydroxy-ethyl acrylate, polymerization inhibitor, disodium ethylene diamine tetraacetate and above-mentioned weight portion heats 30 DEG C and places into mixer
Interior stirring, treats that solid is completely dissolved, and adds urethane acrylate, epoxy acrylate, the precipitation dioxy of above-mentioned weight portion
SiClx, thixotropic agent, hydroxy-ethyl acrylate, trimethylolpropane trimethacrylate, N, accelerine, o-benzoyl sulphonyl are sub-
Amine, coupling agent are well mixed, and are eventually adding isopropyl benzene hydroperoxide.
7. preparation method as claimed in claim 5, it is characterised in that also included before step 2 after the step one：
Step a, the mixed solution is put into reactor, will take out low pressure to 0-10KPa in reactor, is warming up to 20-25 DEG C,
With the Ultrasonic Radiation of 33-35KHz in low pressure and temperature-rise period is taken out, then will recover normal pressure in reactor and be down to room temperature；
Step b, will take out low pressure to 15-20KPa in reactor, be warming up to 25--30 DEG C, and 30- is used in low pressure and temperature-rise period is taken out
The Ultrasonic Radiation of 32KHz, then will recover normal pressure and is down to room temperature in the reactor；
Step c, will take out low pressure to 20-25KPa in reactor, be warming up to 30-35 DEG C, and 25- is used in low pressure and temperature-rise period is taken out
The Ultrasonic Radiation of 28KHz, then will recover normal pressure and to be down to room temperature in the reactor, and to adding 20-40 in reactor
Parts by weight of deionized water.
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| CN201611044370.0A CN106675498A (en) | 2016-11-22 | 2016-11-22 | Anaerobic adhesive and preparation method thereof |
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| CN201611044370.0A CN106675498A (en) | 2016-11-22 | 2016-11-22 | Anaerobic adhesive and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205809A (en) * | 2020-02-27 | 2020-05-29 | 南宁珀源能源材料有限公司 | Rod adhesive for cutting solar silicon wafer and preparation method thereof |
| CN111704887A (en) * | 2020-06-23 | 2020-09-25 | 南雄中科院孵化器运营有限公司 | Thixotropic anaerobic magnetic steel adhesive and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670552A (en) * | 2016-01-26 | 2016-06-15 | 上海都伟光伏科技有限公司 | One-component acrylate structure adhesive with ageing resistance and high-temperature resistance and preparation method of acrylate structure adhesive |
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2016
- 2016-11-22 CN CN201611044370.0A patent/CN106675498A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670552A (en) * | 2016-01-26 | 2016-06-15 | 上海都伟光伏科技有限公司 | One-component acrylate structure adhesive with ageing resistance and high-temperature resistance and preparation method of acrylate structure adhesive |
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| 徐峰: "《建筑涂料与涂装技术》", 31 May 1998, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205809A (en) * | 2020-02-27 | 2020-05-29 | 南宁珀源能源材料有限公司 | Rod adhesive for cutting solar silicon wafer and preparation method thereof |
| CN111704887A (en) * | 2020-06-23 | 2020-09-25 | 南雄中科院孵化器运营有限公司 | Thixotropic anaerobic magnetic steel adhesive and preparation method and application thereof |
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