CN117106392A - High-strength acrylate rapid-curing structural adhesive and preparation method thereof - Google Patents
High-strength acrylate rapid-curing structural adhesive and preparation method thereof Download PDFInfo
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- CN117106392A CN117106392A CN202310976340.7A CN202310976340A CN117106392A CN 117106392 A CN117106392 A CN 117106392A CN 202310976340 A CN202310976340 A CN 202310976340A CN 117106392 A CN117106392 A CN 117106392A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 46
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 46
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 title claims description 31
- 238000002360 preparation method Methods 0.000 title claims description 10
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 25
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000019400 benzoyl peroxide Nutrition 0.000 claims abstract description 24
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 19
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 19
- -1 acrylic ester Chemical class 0.000 claims abstract description 18
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- 239000003112 inhibitor Substances 0.000 claims abstract description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims abstract description 9
- 239000000049 pigment Substances 0.000 claims abstract description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011787 zinc oxide Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 35
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N 1,4-Benzenediol Natural products OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 15
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 14
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 6
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- 150000003512 tertiary amines Chemical class 0.000 claims description 4
- CWRKVLYZMSXVSI-UHFFFAOYSA-N 2-ethyl-n,n-dihydroxy-4-methylaniline Chemical compound CCC1=CC(C)=CC=C1N(O)O CWRKVLYZMSXVSI-UHFFFAOYSA-N 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims description 3
- 229920001897 terpolymer Polymers 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 12
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 238000001723 curing Methods 0.000 description 16
- 238000004519 manufacturing process Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 8
- 239000003292 glue Substances 0.000 description 6
- 125000005396 acrylic acid ester group Chemical group 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000003848 UV Light-Curing Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000000016 photochemical curing Methods 0.000 description 2
- KUBDPQJOLOUJRM-UHFFFAOYSA-N 2-(chloromethyl)oxirane;4-[2-(4-hydroxyphenyl)propan-2-yl]phenol Chemical compound ClCC1CO1.C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 KUBDPQJOLOUJRM-UHFFFAOYSA-N 0.000 description 1
- VALXVSHDOMUUIC-UHFFFAOYSA-N 2-methylprop-2-enoic acid;phosphoric acid Chemical compound OP(O)(O)=O.CC(=C)C(O)=O VALXVSHDOMUUIC-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 239000003522 acrylic cement Substances 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/064—Copolymers with monomers not covered by C09J133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a high-strength acrylic ester rapid curing structural adhesive, which comprises the following components in percentage by mass: 0.5-2 parts of a component A and a component B, wherein the component A is a reducing component, the component B is a zinc oxide component, and the raw materials of the component A comprise the following components in parts by weight based on 100 parts of the sum of the raw materials of the component A: 78-85 parts of polymethyl methacrylate, 10-13 parts of MBS, 3-4 parts of silane coupling agent, 2-3 parts of tertiary amine compound and 1-2 parts of polymerization inhibitor; the raw material composition of the component B comprises 100 parts of the sum of the raw material compositions of the component B: 45-55 parts of dibenzoyl peroxide, 44.5-50 parts of bisphenol A liquid epoxy resin and 0.5-5 parts of pigment blue. Suitable for bonding most metallic and nonmetallic materials; the surface treatment requirements for the adhered materials are not strict, and even the adhered materials can be adhered on the oil surface; high adhesion strength and high impact resistance.
Description
Technical Field
The invention belongs to the technical field of adhesives, and relates to a rapid-curing structural adhesive, in particular to a high-strength acrylic ester rapid-curing structural adhesive and a preparation method thereof.
Background
Acrylic acid esters are the generic term for esters of acrylic acid and its homologs. The acrylic ester adhesive is prepared by taking various acrylic esters as base materials and carrying out chemical reaction, and has the characteristics of light color, water resistance, environmental erosion resistance, good color change resistance and convenient adjustment.
The EASTMAN company in the 50 s of the 20 th century invented the first generation of acrylate adhesives, with benzoyl peroxide/aromatic amine as the redox system, without grafting reaction between the monomer and the elastomer, with the main disadvantage of being brittle. In 1975, duPont invented a 2 nd generation acrylate adhesive (also called a modified acrylate adhesive), the new redox system was made by using peroxide of hydrogen peroxide type as initiator and DuPont 808 aldehyde amine condensate as accelerator; the monomer and the elastomer undergo grafting reaction to form a tough cured product, and the peel strength and impact strength are obviously improved. In 1968, the German Bayer company developed a successful photo-curing coating first, and on the basis of the successful photo-curing coating, a UV curing adhesive (namely a third generation acrylate adhesive) is developed in Europe, and the UV curing coating has the advantages of high curing speed, environmental protection and the like. After that, the acrylic adhesive is gradually industrialized in the 70-80 th century of 20 th year.
At present, the 1 st generation acrylic acid ester glue is rarely applied and basically replaced by the 2 nd generation acrylic acid ester glue; the application field of the 3 rd generation acrylic acid ester glue (UV glue) is greatly different from that of the 2 nd generation acrylic acid ester glue, and a relatively independent system is formed. With the development of global industrialization, the production perfection system of the assembly line is more and more important for production efficiency, and the production efficiency is not only the chip field with strict process requirements, but also the automobile industry with high-strength production; furthermore, the rapid positioning of the components on the production line is also of importance. Therefore, adhesives are being developed to accommodate mass production in an assembly line. Most adhesives existing in the market can meet the requirement of quick curing, but have great defects in the aspects of impact resistance, aging resistance, corrosion resistance and the like.
The Chinese patent application No. 201310509388.3 discloses a high-elasticity room-temperature rapid-curing acrylate structural adhesive and a preparation method thereof, wherein the acrylate structural adhesive consists of A, B components and comprises the following components: the oxidant and the reducing agent, (methyl) acrylic ester monomer or (methyl) acrylic ester oligomer, (methyl) acrylic acid phosphate, toughening tackifier, stabilizer and other auxiliary agents for initiating system polymerization, and the catalyst can also contain plasticizer and epoxy resin. A. The component B is combined according to a certain proportion, and the obtained acrylic structural adhesive has the advantages of high room temperature curing speed, high elongation, good elasticity and wide bonding base materials; but the advantages are mainly reflected in high elongation and good elasticity, and the requirements of high-strength application scenes can not be met.
Disclosure of Invention
Based on the defects, the invention provides the acrylate rapid curing structural adhesive which has good high strength, impact resistance, aging resistance, corrosion resistance and other performances while meeting the requirements of rapid curing.
In order to achieve the above objective, the present invention provides a high-strength acrylate rapid curing structural adhesive, which comprises the following components in mass ratio of 10: 0.5-2 of A component and B component, the A component is reducing component, the B component is zinc oxide component,
the raw material composition of the component A comprises 100 parts of the sum of the raw material compositions of the component A: 78-85 parts of polymethyl methacrylate, 10-13 parts of MBS, 3-4 parts of silane coupling agent, 2-3 parts of tertiary amine compound and 1-2 parts of polymerization inhibitor;
the raw material composition of the component B comprises 100 parts of the sum of the raw material compositions of the component B: 45-55 parts of dibenzoyl peroxide, 44.5-50 parts of bisphenol A liquid epoxy resin and 0.5-5 parts of pigment blue.
Optimally, the preparation method of the polymethyl methacrylate comprises the following steps:
(a) Dissolving 20-30 parts of dibenzoyl peroxide in 100 parts of methyl methacrylate to form a dibenzoyl peroxide solution;
(b) Setting the temperature of the reaction kettle to be 60-110 ℃, adding 75-85 parts of methyl methacrylate, 15-18 parts of acrylic acid and 2-3 parts of tertiary amine, stirring and mixing; and then dropwise adding 2-5 parts of dibenzoyl peroxide solution in 10-20min, and continuing stirring.
Further, in the step (b), the stirring speed of stirring and mixing is 120-180rpm, and the time is 10-15min; the stirring speed of continuous stirring is 220-250rpm, and the time is 10-20min.
Optimally, the MBS is a methyl methacrylate, butadiene and styrene terpolymer.
Optimally, the silane coupling agent is one or a mixture of two selected from KH-560 and KH-550.
Optimally, the tertiary amine compound is a mixture composed of one or more of N-methyldiethanolamine, triethanolamine, N-dimethylaniline, N-dimethylformamide and N, N-dihydroxyethyl-p-methylaniline.
Optimally, the polymerization inhibitor is hydroquinone or p-benzoquinone.
The invention also provides a preparation method of the high-strength acrylate rapid-curing structural adhesive, which comprises the following steps:
(a) Sequentially adding 1-2 parts of polymethyl methacrylate, MBS, silane coupling agent, tertiary amine compound and polymerization inhibitor in the formula amount into a planetary mixer, controlling the vacuum degree to be less than or equal to 0.1MPa, uniformly stirring, and discharging to obtain the component A;
(b) And sequentially adding the dibenzoyl peroxide, the bisphenol A liquid epoxy resin and the pigment blue in the formula amount into a planetary stirrer, stirring, vacuumizing and defoaming, controlling the vacuum degree to be less than or equal to-0.1 MPa, uniformly stirring, and discharging to obtain the component B.
The high-strength acrylic ester rapid curing structural adhesive provided by the invention adopts the specific component A and the specific component B and is mixed according to the specific proportion when in use, so that the structural adhesive can be rapidly cured at room temperature, and is generally in a range of minutes to tens of minutes; can be cured at low temperature, even below 0 ℃; suitable for bonding most metallic and nonmetallic materials; the surface treatment requirements for the adhered materials are not strict, and even the adhered materials can be adhered on the oil surface; high adhesion strength and high impact resistance.
Detailed Description
The invention relates to a high-strength acrylate rapid curing structural adhesive, which comprises the following components in percentage by mass: 0.5-2 of a component A and a component B, wherein the component A is a reducing component, the component B is a zinc oxide component, and the raw materials of the component A comprise the following components in parts by weight based on 100 parts of the sum of the raw materials of the component A: 78-85 parts of polymethyl methacrylate, 10-13 parts of MBS, 3-4 parts of silane coupling agent, 2-3 parts of tertiary amine compound and 1-2 parts of polymerization inhibitor; the raw material composition of the component B comprises 100 parts of the sum of the raw material compositions of the component B: 45-55 parts of dibenzoyl peroxide, 44.5-50 parts of bisphenol A liquid epoxy resin and 0.5-5 parts of pigment blue. By using the specific A-and B-components and mixing them in specific proportions at the time of use, it is possible to cure rapidly at room temperature, typically from a few minutes to a few tens of minutes; can be cured at low temperature, even below 0 ℃; suitable for bonding most metallic and nonmetallic materials; the surface treatment requirements for the adhered materials are not strict, and even the adhered materials can be adhered on the oil surface; high adhesion strength and high impact resistance.
The preparation method of the polymethyl methacrylate comprises the following steps: (a) Dissolving 20-30 parts of dibenzoyl peroxide in 100 parts of methyl methacrylate to form a dibenzoyl peroxide solution; (b) Setting the temperature of the reaction kettle to be 60-110 ℃, adding 75-85 parts of methyl methacrylate, 15-18 parts of acrylic acid and 2-3 parts of tertiary amine, stirring and mixing; and then dropwise adding 2-5 parts of dibenzoyl peroxide solution in 10-20min, and continuing stirring. This allows further control of the molecular weight and thus the formation of a prepolymer of a certain molecular weight. In the step (b), the stirring speed of stirring and mixing is 120-180rpm, and the time is 10-15min; the stirring speed of continuous stirring is 220-250rpm, and the time is 10-20min. The MBS is a terpolymer of methyl methacrylate, butadiene and styrene, and is commercially available. The silane coupling agent is one or two selected from KH-560 and KH-550. The tertiary amine compound is one or a mixture of more of N-methyldiethanolamine, triethanolamine, N-dimethylaniline, N-dimethylformamide and N, N-dihydroxyethyl-p-methylaniline. The polymerization inhibitor is hydroquinone or p-benzoquinone, preferably hydroquinone.
The preparation method of the high-strength acrylate rapid-curing structural adhesive comprises the following steps: (a) Sequentially adding 1-2 parts of polymethyl methacrylate, MBS, silane coupling agent, tertiary amine compound and polymerization inhibitor in the formula amount into a planetary mixer, controlling the vacuum degree to be less than or equal to 0.1MPa, uniformly stirring, and discharging to obtain the component A; (b) Sequentially adding dibenzoyl peroxide, bisphenol A liquid epoxy resin and pigment blue in a formula amount into a planetary stirrer, stirring, vacuumizing and defoaming, controlling the vacuum degree to be less than or equal to-0.1 MPa, uniformly stirring, and discharging after 30min to obtain the component B.
In order that those skilled in the art will better understand the present invention, a technical solution in the embodiments of the present invention will be clearly and completely described in the following, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments obtained under the premise of equivalent changes and modifications made by those skilled in the art based on the embodiments of the present invention shall fall within the scope of the present invention.
Example 1
The embodiment provides a high-strength acrylate rapid curing structural adhesive and a preparation method thereof, and the structural adhesive comprises the following concrete steps: the high-strength acrylate rapid curing structural adhesive comprises the following raw materials in percentage by weight: 1 and B components, wherein the A component is a reducing part and the B component is an oxidizing part.
The raw material composition of the component A comprises, based on 100 parts by weight of the sum of the raw material compositions of the component A (g in the embodiment): 78 parts of polymethyl methacrylate, 13 parts of MBS (EM 500A), 4 parts of KH570, 3 parts of N, N-dimethylaniline and 2 parts of hydroquinone;
the polymethyl methacrylate is prepared by the following method:
(a) Setting the temperature of the reaction kettle to be 100 ℃, adding 80 parts of methyl methacrylate, 15 parts of acrylic acid and 2 parts of tertiary amine into the reaction kettle, setting the stirring speed to be 120rpm, and stirring for 13min until the materials are completely dissolved;
(b) Maintaining the stirring speed, and then dropwise adding 3 parts of dissolved dibenzoyl peroxide (namely, a methyl methacrylate solution of dibenzoyl peroxide, specifically, 100 parts of methyl methacrylate is dissolved and 20 parts of dibenzoyl peroxide is dissolved), wherein the dropwise adding is completed for 15 minutes; and closing the heating device of the reaction kettle, setting the stirring speed to 250rpm, stirring for 10min, and cooling to obtain the polymethyl methacrylate.
The raw materials of the component B comprise 100 parts of the sum of the raw materials of the component B: 52 parts of dibenzoyl peroxide, 47 parts of bisphenol A liquid epoxy resin (Epikote 828) and 1 part of pigment blue.
And (3) preparing a component A: sequentially adding the weighed polymethyl methacrylate, MBS, KH570, tertiary amine compounds and polymerization inhibitor into a planetary mixer, controlling the vacuum degree to be not higher than-0.1 MPa, uniformly stirring, and discharging to obtain a reduced part (namely a component A);
and (3) preparing a component B: sequentially adding dibenzoyl peroxide, bisphenol A liquid epoxy resin and pigment blue into a planetary stirrer, stirring, vacuumizing and defoaming, controlling the vacuum degree to be not higher than-0.1 MPa, uniformly stirring, and discharging after 30min to obtain an oxidized part (namely the component B).
Example 2
This example provides a high strength acrylate rapid cure structural adhesive and method of making same, which is substantially identical to that of example 1, except that:
the raw materials of the component A comprise the following components in parts by weight based on 100 parts of the sum of the raw materials of the component A: 80 parts of polymethyl methacrylate, 13 parts of MBS, 4 parts of KH570, 2 parts of N, N-dimethylaniline and 1 part of hydroquinone.
Example 3
This example provides a high strength acrylate rapid cure structural adhesive and method of making same, which is substantially identical to that of example 1, except that:
the raw material composition of the component A comprises 100 parts of the sum of the raw material compositions of the component A: 84 parts of polymethyl methacrylate, 10 parts of MBS, 3 parts of KH570, 2 parts of N, N-dimethylaniline and 1 part of hydroquinone.
Example 4
This example provides a high strength acrylate rapid cure structural adhesive and method of making same, which is substantially identical to that of example 3, except that: in step (b), 25 parts of dibenzoyl peroxide are dissolved in 100 parts of methyl methacrylate and taken out.
Example 5
This example provides a high strength acrylate rapid cure structural adhesive and method of making same, which is substantially identical to that of example 3, except that: in step (b), 30 parts of dibenzoyl peroxide are dissolved in 100 parts of methyl methacrylate and taken out.
Comparative example 1
Parallel comparison tests were performed on commercially available lotto HHD8540 with the acrylate fast setting adhesive product provided by the present invention.
Comparative example 2
This example provides a high strength acrylate rapid cure structural adhesive and method of making same, which is substantially identical to that of example 1, except that: the weight ratio of the component A to the component B is 10:5.
comparative example 3
This example provides a high strength acrylate rapid cure structural adhesive and method of making same, which is substantially identical to that of example 1, except that: the weight ratio of the component A to the component B is 10:0.2.
comparative example 4
This example provides a high strength acrylate rapid cure structural adhesive and method of making same, which is substantially identical to that of example 1, except that: the raw material composition of the component A comprises, based on 100 parts by weight of the sum of the raw material compositions of the component A (g in the embodiment): 65 parts of polymethyl methacrylate, 22 parts of MBS, 5 parts of KH570, 4 parts of N, N-dimethylaniline and 4 parts of hydroquinone.
Comparative example 5
This example provides a high strength acrylate rapid cure structural adhesive and method of making same, which is substantially identical to that of example 1, except that: the raw material composition of the component A comprises, based on 100 parts by weight of the sum of the raw material compositions of the component A (g in the embodiment): 88 parts of polymethyl methacrylate, 6 parts of MBS, 3 parts of KH570, 2 parts of N, N-dimethylaniline and 1 part of hydroquinone.
Comparative example 6
This example provides a structural adhesive and a method of making the same, which is substantially identical to that of example 1, except that: polymethyl methacrylate was obtained as a commercially available product (Merck average M w 15000by GPC) was powdery, and thus, a glue having uniform properties could not be formed.
The high-strength acrylic quick-setting structural adhesives obtained in examples 1 to 5 and comparative examples 1 to 6 were subjected to performance test (the test standard of shear strength is GB/T7124-2008), and the results thereof are shown in Table 1.
Table 1 table of properties of cured products obtained in examples and comparative examples
Note that: shear strength is tested in GB/T7124-08. The test of the impact strength of the cantilever beam is disclosed in GB/T1843-2008.
The foregoing is merely a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention; while the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (8)
1. A high strength acrylate rapid cure structural adhesive comprising the following components in mass ratio of 10: 0.5-2 of a component A and a component B, wherein the component A is a reducing component, and the component B is a zinc oxide component, and the composition is characterized in that:
the raw material composition of the component A comprises 100 parts of the sum of the raw material compositions of the component A: 78-85 parts of polymethyl methacrylate, 10-13 parts of MBS, 3-4 parts of silane coupling agent, 2-3 parts of tertiary amine compound and 1-2 parts of polymerization inhibitor;
the raw material composition of the component B comprises 100 parts of the sum of the raw material compositions of the component B: 45-55 parts of dibenzoyl peroxide, 44.5-50 parts of bisphenol A liquid epoxy resin and 0.5-5 parts of pigment blue.
2. The high strength acrylate rapid cure structural adhesive of claim 1, wherein the preparation method of polymethyl methacrylate comprises the following steps:
(a) Dissolving 20-30 parts of dibenzoyl peroxide in 100 parts of methyl methacrylate to form a dibenzoyl peroxide solution;
(b) Setting the temperature of a reaction kettle to be 60-110 ℃, adding 75-85 parts of methyl methacrylate, 15-18 parts of acrylic acid and 2-3 parts of tertiary amine, and stirring and mixing; and then dropwise adding 2-5 parts of dibenzoyl peroxide solution in 10-20min, and continuing stirring.
3. The high strength acrylate rapid cure structural adhesive of claim 2, wherein: in the step (b), the stirring speed of stirring and mixing is 120-180rpm, and the time is 10-15min; the stirring speed of continuous stirring is 220-250rpm, and the time is 10-20min.
4. The high strength acrylate rapid cure structural adhesive of claim 1, wherein: the MBS is a terpolymer of methyl methacrylate, butadiene and styrene.
5. The high strength acrylate rapid cure structural adhesive of claim 1, wherein: the silane coupling agent is one or two selected from KH-560 and KH-550.
6. The high strength acrylate rapid cure structural adhesive of claim 1, wherein: the tertiary amine compound is one or a mixture of more of N-methyldiethanolamine, triethanolamine, N-dimethylaniline, N-dimethylformamide and N, N-dihydroxyethyl-p-methylaniline.
7. The high strength acrylate rapid cure structural adhesive of claim 1, wherein: the polymerization inhibitor is hydroquinone or p-benzoquinone.
8. A method for preparing the high strength acrylate rapid cure structural adhesive of any one of claims 1 to 7 comprising the steps of:
(a) Sequentially adding 1-2 parts of polymethyl methacrylate, MBS, silane coupling agent, tertiary amine compound and polymerization inhibitor in the formula amount into a planetary mixer, controlling the vacuum degree to be less than or equal to 0.1MPa, uniformly stirring, and discharging to obtain the component A;
(b) And sequentially adding the dibenzoyl peroxide, the bisphenol A liquid epoxy resin and the pigment blue in the formula amount into a planetary stirrer, stirring, vacuumizing and defoaming, controlling the vacuum degree to be less than or equal to-0.1 MPa, uniformly stirring, and discharging to obtain the component B.
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