CN105542692A - Method for producing copper foil glue for paper-based copper clad laminate - Google Patents
Method for producing copper foil glue for paper-based copper clad laminate Download PDFInfo
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- CN105542692A CN105542692A CN201510951816.7A CN201510951816A CN105542692A CN 105542692 A CN105542692 A CN 105542692A CN 201510951816 A CN201510951816 A CN 201510951816A CN 105542692 A CN105542692 A CN 105542692A
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- copper foil
- paper
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- foil glue
- copper
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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
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C09J161/04, C09J161/18 and C09J161/20
-
- 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
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/12—Chemically modified polycondensates
-
- 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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Laminated Bodies (AREA)
- Manufacturing Of Printed Wiring (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention discloses a method for producing a copper foil glue for a paper-based copper clad laminate. The method is as follows: step 1, synthesis of modified barium phenolic resin: 1) adding 2350-2450 parts of phenol, 3000-3200 parts of formaldehyde and 120-140 parts of melamine formaldehyde resin to a reaction vessel, adding 25-28 parts of barium hydroxide under stirring, and heating for reaction; 2) after the reaction, vacuumizing, reducing pressure, dehydrating, adding 380-2300 parts of a solvent, stirring and cooling for standby; step 2, mixing and dissolving 240-260 parts of the obtained modified barium phenolic resin with 150-160 parts of polyvinyl butyral and 18-22 parts of base epoxy resin in 1090-1310 parts of an organic solvent to obtain the copper foil glue. The produced copper foil glue significantly improves the peel strength and uniformity of the peel strength of the copper clad laminate, and can be applied to production of thin copper foil paper-based copper clad laminate to achieved good economic benefits.
Description
Technical field
The present invention relates to paper-based copper-coated board and manufacture field, specifically refer to a kind of manufacture method of paper-based copper-coated board Copper Foil glue.
Background technology
Paper-based copper-coated board manufactures alligatoring Copper Foil used, with prepreg hot pressing cladding before first must be coated with one deck Copper Foil sizing agent, to meet the requirement of the resistance to dip solderability and stripping strength of copper-clad plate product.By in the environment exposed for paper fiber after Copper Foil etching simultaneously when sizing agent can also be avoided making wiring board, strengthen water-intake rate, reduce insulation resistance, cause circuit card to lose efficacy.Therefore, Copper Foil sizing agent formula and manufacturing process thereof are the important component parts of paper-based copper-coated board production technology.Copper-clad plate production Copper Foil is to slimming future development, and traditional paper-based copper-coated board Copper Foil is based on 35um thickness, and current 18um thickness Copper Foil is occupied an leading position.15um, 13um thickness Copper Foil increases year by year in the usage ratio of paper-based copper-coated board in recent years.Along with the minimizing of copper thickness, the roughened layer thickness of adhesive surface is also in minimizing, and the stripping strength of product is affected, and in electronic product assembling process, easily copper sheet obscission occurs, cause product rejection, financial loss is serious.How improving the stripping strength of thin copper foil or extra thin copper foil paper-based copper-coated board, improve the reliability of electronic product, is the problem that paper-based copper-coated board production firm is concerned about.
Summary of the invention
The object of the present invention is to provide a kind of manufacture method of paper-based copper-coated board Copper Foil glue, obtained Copper Foil glue significantly improves the stripping strength of copper-clad plate and the homogeneity of stripping strength, in producing for slim Copper Foil paper-based copper-coated board, achieve good economic benefit.
In order to reach above-mentioned purpose, solution of the present invention is:
A manufacture method for paper-based copper-coated board Copper Foil glue, its step is as follows:
The synthesis of step one, modification ba phenolic resin
1) in reactor, add the terpolycyantoamino-formaldehyde resin of the phenol of 2350-2450 part, the formaldehyde of 3000-3200 part and 120-140 part, adding the hydrated barta of 25-28 part when stirring, carrying out temperature reaction afterwards;
2), after reaction terminates, vacuumize decompression dehydration, add the solvent of 380-2300 part after completing, stir afterwards and cool, lay in stand-by;
Step 2, by the base epoxy resin of the polyvinyl butyral acetal of the modification ba phenolic resin of obtained 240-260 part and 150-160 part, 18-22 part mixed dissolution in the organic solvent of 1090-1310 part, Copper Foil glue of the present invention can be obtained;
Described part is weight part.
1 of described step one) in carry out temperature reaction, from beginning to warm to 80 DEG C, the time is 15 ± 5 minutes; Carry out nature intensification when temperature rises to 80 DEG C, calculating reacting time when being warming up to 90 DEG C, the reaction times is 60 minutes, keeps temperature 100 DEG C.
2 of described step one) in, reaction terminates decompression dehydration immediately, and in 5 minutes, vacuum tightness reaches 0.03Mpa, and final vacuum tightness is 0.08-0.09 (5-10 divides) Mpa; The large heating of steam when temperature is down to 70 DEG C, vapour pressure is less than 0.5Mpa; When dehydration temperaturre is gone up to 75 DEG C, gel time is surveyed in sampling, reaches 90-110 second (160 DEG C), and stopping vacuumizes and adds the solvent of 380-2300 part.
2 of described step one) in, solvent is the vinyl acetic monomer of 380-400 part and the methyl alcohol of 1700-1900 part.
In described step 2, first adding in dissolving vessel by the organic solvent of 1090-1310 part, adding the polyvinyl butyral acetal of 150-160 part when stirring, stirring and dissolving is until dissolve completely; Add the modification ba phenolic resin of 240-260 part and the base epoxy resin of 18-22 part afterwards, continue stirring and dissolving, be i.e. obtained Copper Foil glue of the present invention.
In described step 2, organic solvent is the methyl alcohol of 1000-1200 part and the acetone of 90-110 part.
After adopting such scheme, the manufacture method of a kind of paper-based copper-coated board Copper Foil of the present invention glue, synthesize a kind of terpolycyantoamino-formaldehyde resin modification ba phenolic resin, by the ba phenolic resin of modification and polyvinyl butyral acetal, base epoxy resin mixed dissolution in organic solvent, make Copper Foil glue, the stripping strength of copper-clad plate and the homogeneity of stripping strength can be significantly improved.
By the cyanurotriamide modified ba phenolic resin obtained by preparation method of the present invention, owing to introducing stable heterocycle structure, and the cross-linking density of resin improves, and can significantly improve the thermotolerance of resin, heat decomposition temperature as phenolic resin is 380 DEG C, is 438 DEG C after cyanurotriamide modified.In electronic product assembling process, be not easy to occur the defects such as layering, foaming, Copper Foil come off.In addition, cyanurotriamide modified ba phenolic resin, system polar groups increases, because metal or metal oxide surface are all high energy surface, the sizing agent of strong polarity, to the easy spreading wetting of copper foil surface, improves cohesive strength, improve the stripping strength of Copper Foil, and improve the homogeneity of stripping strength.In producing for slim Copper Foil paper-based copper-coated board, achieve good economic benefit.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
The present invention relates to a kind of manufacture method of paper-based copper-coated board Copper Foil glue, its step is as follows:
The synthesis of step one, modification ba phenolic resin
1) in reactor, add the terpolycyantoamino-formaldehyde resin of the phenol of 2350-2450 part, the formaldehyde of 3000-3200 part and 120-140 part, adding the hydrated barta of 25-28 part when stirring, carrying out temperature reaction afterwards;
Described phenol, formaldehyde and terpolycyantoamino-formaldehyde resin to be sequentially added in reactor and to stir, and add hydrated barta when stirring, and stir beginning temperature reaction in 3-5 minute;
Described temperature reaction, concrete operations embodiment is, from beginning to warm to 80 DEG C, the time is 15 ± 5 minutes; When temperature rises to 80 DEG C, close porthole and make it naturally heat up, calculating reacting time when being warming up to 90 DEG C, the reaction times is 60 minutes, maintenance temperature 100 DEG C.
2), after reaction terminates, vacuumize decompression dehydration, add the solvent of 380-2300 part after completing, stir afterwards and cool, lay in stand-by; Described solvent one preferred embodiment is the vinyl acetic monomer of 380-400 part and the methyl alcohol of 1700-1900 part.
Described reaction terminates decompression dehydration immediately, and concrete operations embodiment is, in 5 minutes, vacuum tightness reaches 0.03Mpa, and final vacuum tightness is 0.08-0.09 (5-10 divides) Mpa; Open the large heating of steam when temperature is down to 70 DEG C, vapour pressure is less than 0.5Mpa; When dehydration temperaturre is gone up to 75 DEG C, gel time is surveyed in sampling, reaches 90-110 second (160 DEG C), and stopping vacuumizes and adds the solvent of 380-2300 part; Solvent adds rear stirring, is cooled to 40 DEG C, stops stirring deposit stand-by.
Shown in the synthetic materials of described modification ba phenolic resin and proportioning form specific as follows.
| Sequence number | Starting material title | Specification | Charging capacity (kg) |
| 1 | Phenol | Industry one-level | 2350-2450 |
| 2 | Formaldehyde | 37％ | 3000-3200 |
| 3 | Terpolycyantoamino-formaldehyde resin | 45％ | 120-140 |
| 4 | Hydrated barta | C.P | 25-28 |
| 5 | Vinyl acetic monomer | Qualified | 380-400 |
| 6 | Methyl alcohol | Qualified | 1700-1900 |
For synthetic materials and the proportioning of modification ba phenolic resin, provide shown in the following form of a specific embodiment.
| Sequence number | Starting material title | Specification | Charging capacity (kg) |
| 1 | Phenol | Industry one-level | 2400 |
| 2 | Formaldehyde | 37％ | 3150 |
| 3 | Terpolycyantoamino-formaldehyde resin | 45％ | 120 |
| 4 | Hydrated barta | C.P | 27 |
| 5 | Vinyl acetic monomer | Qualified | 396 |
| 6 | Methyl alcohol | Qualified | 1800 |
Synthesized obtained modification ba phenolic resin, quality index is with reference to shown in lower form.
| Test item | Testing conditions | Examination criteria |
| Outward appearance | Room temperature | Red-brown transparent liquid |
| Gel time | 160±2℃ | 60-80 second |
| Solids content | 140℃ 1H | 52-56％ |
Step 2, by the base epoxy resin of the polyvinyl butyral acetal of the modification ba phenolic resin of obtained 240-260 part and 150-160 part, 18-22 part mixed dissolution in the organic solvent of 1090-1310 part, Copper Foil glue of the present invention can be obtained.This organic solvent preferred embodiment is the methyl alcohol of 1000-1200 part and the acetone of 90-110 part.
Dissolving operation steps optimal way is, first the organic solvent of 1090-1310 part is added in (successively adding methyl alcohol and acetone in order) dissolving vessel, the polyvinyl butyral acetal of 150-160 part is added when stirring, stirring and dissolving is until dissolve completely, and the stirring and dissolving time is preferably no less than 8 hours; Add the modification ba phenolic resin of 240-260 part and the base epoxy resin of 18-22 part afterwards, continue stirring and dissolving (dissolving 1 hour), released by glue afterwards, sampling and testing, conformance with standard i.e. obtained Copper Foil glue of the present invention also uses.
Above-described part is weight part.
Shown in the starting material of described Copper Foil glue preparation and the following form of proportioning.
| Sequence number | Starting material title | Specification | Charging capacity (kg) |
| 1 | Methyl alcohol | Qualified | 1000-1200 |
| 2 | Acetone | Qualified | 90-110 |
| 3 | Polyvinyl butyral acetal | Qualified | 150-160 |
| 4 | Modification ba phenolic resin | 50％ | 240-260 |
| 5 | Base epoxy resin | Qualified | 18-22 |
For starting material and the proportioning of the preparation of Copper Foil glue, provide shown in the following form of a specific embodiment.
| Sequence number | Starting material title | Specification | Charging capacity (kg) |
| 1 | Methyl alcohol | Qualified | 1150 |
| 2 | Acetone | Qualified | 100 |
| 3 | Polyvinyl butyral acetal | Qualified | 150 |
| 4 | Modification ba phenolic resin | 50％ | 250 |
| 5 | Base epoxy resin | Qualified | 20 |
Synthesized obtained Copper Foil glue, quality index is with reference to shown in lower form.
| Sequence number | Project name | Standard |
| 1 | Outward appearance | Yellow or amber transparent liquid |
| 2 | Solids content (150 DEG C, 1 hour) | 17-20％ |
The Copper Foil glue application example that the present invention obtains is as follows: be coated on the alligatoring Copper Foil of 15um or 12um thickness by the Copper Foil glue prepared above, at 140-16 DEG C, drying is except desolventizing, and controlling acetone soluble 20-30%, Amount of spread every square metre 14g-16g, makes adhesive coated foil.With 1 adhesive coated foil and 8 paper substrate prepregs superimposed, at 100Kg/cm
2, hot pressing 100 minutes under 160 DEG C of conditions, namely makes the copper-clad laminate that thickness is 1.6mm.Resistance to dip solderability (260 DEG C) more than 15 seconds of sheet material, stripping strength 1.2-1.4N/mm, other performances reach CPFCP-04 technical requirement in GB4723-92 standard.
The foregoing is only the preferred embodiments of the present invention, all equalizations done with the claims in the present invention scope change and modify, and all should belong to the scope of the claims in the present invention.
Claims (6)
1. a paper-based copper-coated board manufacture method for Copper Foil glue, it is characterized in that, step is as follows:
The synthesis of step one, modification ba phenolic resin
1) in reactor, add the terpolycyantoamino-formaldehyde resin of the phenol of 2350-2450 part, the formaldehyde of 3000-3200 part and 120-140 part, adding the hydrated barta of 25-28 part when stirring, carrying out temperature reaction afterwards;
2), after reaction terminates, vacuumize decompression dehydration, add the solvent of 380-2300 part after completing, stir afterwards and cool, lay in stand-by;
Step 2, by the base epoxy resin of the polyvinyl butyral acetal of the modification ba phenolic resin of obtained 240-260 part and 150-160 part, 18-22 part mixed dissolution in the organic solvent of 1090-1310 part, Copper Foil glue of the present invention can be obtained;
Described part is weight part.
2. the manufacture method of a kind of paper-based copper-coated board Copper Foil glue as claimed in claim 1, is characterized in that, 1 of described step one) in carry out temperature reaction, from beginning to warm to 80 DEG C, the time is 15 ± 5 minutes; Carry out nature intensification when temperature rises to 80 DEG C, calculating reacting time when being warming up to 90 DEG C, the reaction times is 60 minutes, keeps temperature 100 DEG C.
3. the manufacture method of a kind of paper-based copper-coated board Copper Foil glue as claimed in claim 1, it is characterized in that, 2 of described step one) in, reaction terminates decompression dehydration immediately, in 5 minutes, vacuum tightness reaches 0.03Mpa, and final vacuum tightness is that 0.08-0.09(5-10 divides) Mpa; The large heating of steam when temperature is down to 70 DEG C, vapour pressure is less than 0.5Mpa; When dehydration temperaturre is gone up to 75 DEG C, gel time is surveyed in sampling, reaches 90-110 second (160 DEG C), and stopping vacuumizes and adds the solvent of 380-2300 part.
4. the manufacture method of a kind of paper-based copper-coated board Copper Foil glue as described in claim 1 or 3, is characterized in that, 2 of described step one) in, solvent is the vinyl acetic monomer of 380-400 part and the methyl alcohol of 1700-1900 part.
5. the manufacture method of a kind of paper-based copper-coated board Copper Foil glue as claimed in claim 1, it is characterized in that, in described step 2, first the organic solvent of 1090-1310 part is added in dissolving vessel, add the polyvinyl butyral acetal of 150-160 part when stirring, stirring and dissolving is until dissolve completely; Add the modification ba phenolic resin of 240-260 part and the base epoxy resin of 18-22 part afterwards, continue stirring and dissolving, be i.e. obtained Copper Foil glue of the present invention.
6. the manufacture method of a kind of paper-based copper-coated board Copper Foil glue as described in claim 1 or 5, is characterized in that, in described step 2, organic solvent is the methyl alcohol of 1000-1200 part and the acetone of 90-110 part.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810650356.8A CN109082252B (en) | 2015-12-17 | 2015-12-17 | Copper foil adhesive for high-peel-strength paper-based copper-clad plate |
| CN201510951816.7A CN105542692B (en) | 2015-12-17 | 2015-12-17 | A kind of manufacturing method of paper-based copper-coated board copper foil glue |
| CN201810649919.1A CN108977144B (en) | 2015-12-17 | 2015-12-17 | Method for manufacturing copper foil adhesive for thin paper-based copper-clad plate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510951816.7A CN105542692B (en) | 2015-12-17 | 2015-12-17 | A kind of manufacturing method of paper-based copper-coated board copper foil glue |
Related Child Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810650356.8A Division CN109082252B (en) | 2015-12-17 | 2015-12-17 | Copper foil adhesive for high-peel-strength paper-based copper-clad plate |
| CN201810649919.1A Division CN108977144B (en) | 2015-12-17 | 2015-12-17 | Method for manufacturing copper foil adhesive for thin paper-based copper-clad plate |
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| Publication Number | Publication Date |
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| CN105542692A true CN105542692A (en) | 2016-05-04 |
| CN105542692B CN105542692B (en) | 2018-08-03 |
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| CN201510951816.7A Active CN105542692B (en) | 2015-12-17 | 2015-12-17 | A kind of manufacturing method of paper-based copper-coated board copper foil glue |
| CN201810650356.8A Active CN109082252B (en) | 2015-12-17 | 2015-12-17 | Copper foil adhesive for high-peel-strength paper-based copper-clad plate |
| CN201810649919.1A Active CN108977144B (en) | 2015-12-17 | 2015-12-17 | Method for manufacturing copper foil adhesive for thin paper-based copper-clad plate |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810650356.8A Active CN109082252B (en) | 2015-12-17 | 2015-12-17 | Copper foil adhesive for high-peel-strength paper-based copper-clad plate |
| CN201810649919.1A Active CN108977144B (en) | 2015-12-17 | 2015-12-17 | Method for manufacturing copper foil adhesive for thin paper-based copper-clad plate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113388349A (en) * | 2021-05-13 | 2021-09-14 | 福建利豪电子科技股份有限公司 | Preparation process of copper foil adhesive special for high CTI (comparative tracking index) and application of copper foil adhesive to paper-based copper-clad plate |
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| CN113388349A (en) * | 2021-05-13 | 2021-09-14 | 福建利豪电子科技股份有限公司 | Preparation process of copper foil adhesive special for high CTI (comparative tracking index) and application of copper foil adhesive to paper-based copper-clad plate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108977144B (en) | 2021-01-08 |
| CN108977144A (en) | 2018-12-11 |
| CN109082252A (en) | 2018-12-25 |
| CN105542692B (en) | 2018-08-03 |
| CN109082252B (en) | 2021-01-08 |
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