CN112175559A - Formula and preparation method of high-temperature-resistant, high-strength and high-toughness epoxy resin adhesive - Google Patents
Formula and preparation method of high-temperature-resistant, high-strength and high-toughness epoxy resin adhesive Download PDFInfo
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- CN112175559A CN112175559A CN202010614625.2A CN202010614625A CN112175559A CN 112175559 A CN112175559 A CN 112175559A CN 202010614625 A CN202010614625 A CN 202010614625A CN 112175559 A CN112175559 A CN 112175559A
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- epoxy resin
- strength
- temperature
- resin adhesive
- resistant
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
Abstract
The invention discloses a high-temperature-resistant high-strength high-toughness epoxy resin adhesive formula which comprises 100 (10-20) parts by mass of rubber modified bisphenol F base resin, 1-10 parts by mass of dicyandiamide curing agent and accelerator; also discloses a preparation method of the high-temperature-resistant high-strength high-toughness epoxy resin adhesive, which comprises the following steps: s1, pouring the rubber modified bisphenol F base resin, the dicyandiamide curing agent and the accelerator into a container in sequence and mixing uniformly; s2, heating and mixing the mixture in an oven; s3, adding a proper amount of pigment; s4, repeatedly grinding the mixture for multiple times; s5, putting the mixture into an oven to bake to remove resin impurities; s6, vacuumizing for 1-2 hours, discharging and cooling; the epoxy resin adhesive has the advantages of high temperature resistance, good toughness, no halogen and high strength resistance, can be used for scrapping and grafting of PCBs, reduces scrapping of PCBs, reduces purchasing cost of SMT circuit boards, and has wide application value.
Description
Technical Field
The invention relates to an epoxy resin adhesive, in particular to a high-temperature-resistant high-strength high-toughness epoxy resin adhesive formula and a preparation method thereof.
Background
In order to provide the PCB transplanting plate with good high temperature resistance, epoxy glue containing multifunctional resin is generally used. The existing multifunctional resin is very brittle and low in bonding strength although being heat-resistant, and cannot pass a drop test when being used for a PCB transplanting plate, and in addition, the multifunctional resin has high halogen and cannot meet safety indexes.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a formula of a high-temperature-resistant, high-strength and high-toughness epoxy resin adhesive which has good high-temperature-resistant performance and toughness, is halogen-free and high-strength-resistant and can be used for a scrapped PCB grafting process, and also provides a preparation method of the high-temperature-resistant, high-strength and high-toughness epoxy resin adhesive.
In order to achieve the purpose, the invention provides a high-temperature-resistant high-strength high-toughness epoxy resin adhesive formula which comprises 100 (10-20) parts by mass of rubber modified bisphenol F base resin, 1-10 parts by mass of dicyandiamide curing agent and accelerator.
Preferably, the color adjusting agent further comprises a pigment for adjusting the color of a sample, and the mass fraction ratio of the pigment to the rubber modified bisphenol F base resin is (1-8): 100.
preferably, the accelerator is UR 300.
Compared with the prior art, the formula of the high-temperature-resistant high-strength high-toughness epoxy resin adhesive provided by the invention has the beneficial effects that:
the epoxy resin adhesive has the advantages of good high temperature resistance, good toughness, no halogen and high strength resistance, can be used for the scrapped grafting process of the PCB, reduces the scrapping of a PCB transplant board, reduces the purchase cost of an SMT circuit board, and has wide application value.
The invention also provides a preparation method of the high-temperature-resistant high-strength high-toughness epoxy resin adhesive, which comprises the following steps:
s1, pouring 100 parts by mass of rubber modified bisphenol F base resin, 10-20 parts by mass of dicyandiamide curing agent and 1-10 parts by mass of accelerator into a container in sequence, and premixing to ensure that all the formulas are well and uniformly blended;
s2, after being uniformly mixed in the step S1, the mixture is put into an oven to be heated to 50-80 ℃, and is heated and mixed under the condition of 50-80 ℃, so that the adhesion degree of the glue is improved;
s3, heating and mixing in the step S2, and then adding a proper amount of pigment into the mixture;
s4, adding the pigment for color matching in the step S3, then gluing the pigment into a grinding machine, adjusting the speed of the grinding machine, and repeatedly grinding the pigment for multiple times to improve the solubility and the viscosity;
s5, repeatedly grinding the mixture for multiple times by the grinder in the step S4, putting the mixture into a container, and baking the container in an oven to remove resin impurities;
s6, after removing resin impurities in the step S5, putting the epoxy resin glue into a vacuum defoaming machine, vacuumizing for 1-2 hours, discharging and cooling to obtain the high-temperature-resistant high-strength high-toughness epoxy resin glue.
Preferably, the viscosity of the rubber modified bisphenol F base resin in the step S1 is 4.5-5.0 Pa.s at 25 ℃, and the epoxy content is 190 g/eq.
Preferably, the accelerator in step S1 is UR 300.
Preferably, the heating and kneading time in the oven in step S2 is 1 to 2 hours.
Preferably, the grinding speed of the grinder in the step S4 is 30 m/min, and the number of grinding times is four.
Preferably, the temperature of the oven in step S5 is 50 ° and the baking time is 1 hour.
Compared with the prior art, the preparation method of the high-temperature-resistant high-strength high-toughness epoxy resin adhesive provided by the invention has the beneficial effects that:
the epoxy resin adhesive prepared by the heating forming method has the advantages of good high temperature resistance, good toughness, no halogen and high strength resistance, can be used for a scrapped PCB grafting process, reduces scrapping of PCB transplanting plates, reduces purchasing cost of SMT circuit boards, and has wide application value.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The invention provides a high-temperature-resistant high-strength high-toughness epoxy resin adhesive formula which comprises 100 (10-20) parts by mass of rubber modified bisphenol F base resin, 1-10 parts by mass of dicyandiamide curing agent and accelerator, wherein the epoxy resin adhesive formula also comprises a proper amount of pigment for adjusting the color of a sample, and the mass fraction ratio of the pigment to the rubber modified bisphenol F base resin is (1-8): 100, in the present embodiment, the promoter is preferably UR 300. The epoxy resin adhesive has the advantages of good high temperature resistance, good toughness, no halogen and high strength resistance, can be used for the scrapped grafting process of the PCB, reduces the scrapping of a PCB transplant board, reduces the purchase cost of an SMT circuit board, and has wide application value.
Example two
The invention also provides a preparation method of the high-temperature-resistant high-strength high-toughness epoxy resin adhesive, which comprises the following steps:
s1, pouring 100 parts by mass of rubber modified bisphenol F base resin, 10-20 parts by mass of dicyandiamide curing agent and 1-10 parts by mass of accelerator into a stainless steel container in sequence, and premixing to ensure that all the formulas are well and uniformly blended;
wherein in step S1: the viscosity of the rubber modified bisphenol F base resin at 25 ℃ is 4.5-5.0 Pa.s, and the epoxy 175-190 g/eq; the accelerant is UR 300;
s2, after the step S1 of uniform mixing, putting the mixture into an oven to be heated to 50-80 ℃, and heating and mixing for 1-2 hours at the temperature of 50-80 ℃ to improve the adhesion degree of the glue;
s3, heating and mixing in the step S2, and then adding a proper amount of pigment into the mixture;
s4, adding the pigment for color matching in the step S3, then gluing the pigment into a grinding machine, adjusting the speed of the grinding machine, and repeatedly grinding the pigment for multiple times to improve the solubility and the viscosity;
wherein in step S4: the grinding speed of the grinder is 30 m/min, and the grinding times are preferably four times;
s5, repeatedly grinding the mixture for multiple times by the grinder in the step S4, putting the mixture into a container, and baking the container in an oven to remove resin impurities;
wherein in step S5: the temperature of the oven is 50 degrees, and the baking time is 1 hour;
s6, after removing resin impurities in the step S5, putting the epoxy resin glue into a vacuum defoaming machine, vacuumizing for 1-2 hours, discharging and cooling to obtain the high-temperature-resistant high-strength high-toughness epoxy resin glue.
And (3) carrying out PCB transplantation plate glue injection experiment on the epoxy resin glue subjected to the colloid vacuum removal in the step S6: injecting high-temperature glue into the transplanting gap by a glue dispenser, and baking according to conditions (110 degrees/30 minutes-130 degrees/60 minutes).
The epoxy resin adhesive is subjected to a tensile test experiment, a drop test experiment and a deflection test experiment, as shown in the following table, 10 groups of comparison data of the epoxy resin adhesive and the common adhesive provided by the invention under the condition that the same bonding cross section area is 20 square millimeters are shown, the following table shows that the garbage value of the common adhesive at 250 ℃ is 0KG, so that the common adhesive has extremely poor high temperature resistance, and the epoxy resin adhesive prepared by the heating forming method has the advantages of good high temperature resistance, good toughness, no halogen and high strength resistance, can be used for a PCB scrapping and grafting process, reduces scrapping of PCB transplanted plates, reduces purchasing cost of SMT circuit boards, and has wide application value.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. The formula of the high-temperature-resistant high-strength high-toughness epoxy resin adhesive is characterized by comprising 100 (10-20) parts by mass of rubber modified bisphenol F base resin, 1-10 parts by mass of dicyandiamide curing agent and accelerator.
2. The formula of the high-temperature-resistant, high-strength and high-toughness epoxy resin adhesive as claimed in claim 1, further comprising a pigment for adjusting the color of a sample, wherein the mass fraction ratio of the pigment to the rubber-modified bisphenol F base resin is (1-8): 100.
3. the formulation of claim 1, wherein the accelerator is UR 300.
4. The preparation method of the high-temperature-resistant high-strength high-toughness epoxy resin adhesive is characterized by comprising the following steps of:
s1, pouring 100 parts by mass of rubber modified bisphenol F base resin, 10-20 parts by mass of dicyandiamide curing agent and 1-10 parts by mass of accelerator into a container in sequence, and premixing to ensure that all the formulas are well and uniformly blended;
s2, after being uniformly mixed in the step S1, the mixture is put into an oven to be heated to 50-80 ℃, and is heated and mixed under the condition of 50-80 ℃, so that the adhesion degree of the glue is improved;
s3, heating and mixing in the step S2, and then adding a proper amount of pigment into the mixture;
s4, adding the pigment for color matching in the step S3, then gluing the pigment into a grinding machine, adjusting the speed of the grinding machine, and repeatedly grinding the pigment for multiple times to improve the solubility and the viscosity;
s5, repeatedly grinding the mixture for multiple times by the grinder in the step S4, putting the mixture into a container, and putting the container into an oven to bake resin impurities;
s6, after removing resin impurities in the step S5, putting the epoxy resin glue into a vacuum defoaming machine, vacuumizing for 1-2 hours, discharging and cooling to obtain the high-temperature-resistant high-strength high-toughness epoxy resin glue.
5. The method for preparing the high temperature resistant, high strength and high toughness epoxy resin adhesive according to claim 4, wherein the viscosity of the rubber modified bisphenol F base resin in the step S1 is 4.5 to 5.0Pa.s at 25 ℃, and the epoxy content is 175-190 g/eq.
6. The method for preparing the high temperature resistant, high strength and high toughness epoxy resin adhesive according to claim 4, wherein the accelerator in step S1 is UR 300.
7. The method for preparing the high temperature resistant, high strength and high toughness epoxy resin adhesive according to claim 4, wherein the heating and mixing time in the oven in step S2 is 1-2 hours.
8. The method for preparing the epoxy resin adhesive with high temperature resistance, high strength and high toughness as claimed in claim 4, wherein the grinding speed of the grinder in step S4 is 30 m/min, and the grinding times are four times.
9. The method for preparing the high temperature resistant, high strength and high toughness epoxy resin adhesive according to claim 4, wherein the temperature of the oven at step S5 is 50 ° and the baking time is 1 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010614625.2A CN112175559A (en) | 2020-06-30 | 2020-06-30 | Formula and preparation method of high-temperature-resistant, high-strength and high-toughness epoxy resin adhesive |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010614625.2A CN112175559A (en) | 2020-06-30 | 2020-06-30 | Formula and preparation method of high-temperature-resistant, high-strength and high-toughness epoxy resin adhesive |
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| Publication Number | Publication Date |
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| CN112175559A true CN112175559A (en) | 2021-01-05 |
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| CN202010614625.2A Pending CN112175559A (en) | 2020-06-30 | 2020-06-30 | Formula and preparation method of high-temperature-resistant, high-strength and high-toughness epoxy resin adhesive |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760161A (en) * | 2008-12-24 | 2010-06-30 | 深圳市道尔科技有限公司 | Environmental-protection low halogen-content surface mounting adhesive capable of quick solidification under low temperature |
| US20140113983A1 (en) * | 2011-02-15 | 2014-04-24 | Zephyros Inc. | Structural adhesives |
| CN105315945A (en) * | 2014-07-25 | 2016-02-10 | 上海腾烁电子材料有限公司 | Anisotropic electric conductivity adhesive and preparation method thereof |
| CN108137858A (en) * | 2015-10-20 | 2018-06-08 | Ppg工业俄亥俄公司 | structural adhesive composition |
| CN110050052A (en) * | 2016-10-24 | 2019-07-23 | 陶氏环球技术有限责任公司 | It is resistant to the epoxy adhesive of open pearl humidity exposure |
-
2020
- 2020-06-30 CN CN202010614625.2A patent/CN112175559A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760161A (en) * | 2008-12-24 | 2010-06-30 | 深圳市道尔科技有限公司 | Environmental-protection low halogen-content surface mounting adhesive capable of quick solidification under low temperature |
| US20140113983A1 (en) * | 2011-02-15 | 2014-04-24 | Zephyros Inc. | Structural adhesives |
| CN105315945A (en) * | 2014-07-25 | 2016-02-10 | 上海腾烁电子材料有限公司 | Anisotropic electric conductivity adhesive and preparation method thereof |
| CN108137858A (en) * | 2015-10-20 | 2018-06-08 | Ppg工业俄亥俄公司 | structural adhesive composition |
| CN110050052A (en) * | 2016-10-24 | 2019-07-23 | 陶氏环球技术有限责任公司 | It is resistant to the epoxy adhesive of open pearl humidity exposure |
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Application publication date: 20210105 |