CN105542692B - A kind of manufacturing method of paper-based copper-coated board copper foil glue - Google Patents
A kind of manufacturing method of paper-based copper-coated board copper foil glue Download PDFInfo
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- CN105542692B CN105542692B CN201510951816.7A CN201510951816A CN105542692B CN 105542692 B CN105542692 B CN 105542692B CN 201510951816 A CN201510951816 A CN 201510951816A CN 105542692 B CN105542692 B CN 105542692B
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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
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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
- 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
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- 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
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- 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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- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Laminated Bodies (AREA)
- Manufacturing Of Printed Wiring (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention discloses a kind of manufacturing method of paper-based copper-coated board copper foil glue, and steps are as follows:Step 1: the synthesis of modified ba phenolic resin:1)In 2,350 2450 parts of phenol, 3,000 3200 parts of formaldehyde and 120 140 parts of melamine resin are added in reaction kettle, 25 28 parts of barium hydroxide is added in the case of stirring, carries out temperature reaction later;2)After reaction, decompression dehydration is vacuumized, 380 2300 parts of solvent is added after the completion, is stirred later and cooling, deposit is for use;Step 2: by obtained 240 260 parts of modification ba phenolic resin and 150 160 parts of polyvinyl butyral, 18 22 parts of base epoxy resin mixed dissolution in 1,090 1310 parts of organic solvent, you can copper foil glue of the present invention is made.Copper foil glue obtained significantly improves the peel strength of copper-clad plate and the uniformity of peel strength, in the production of slim copper foil paper-based copper-coated board, achieving preferable economic benefit.
Description
Technical field
The present invention relates to paper-based copper-coated board manufacturing field, in particular to a kind of manufacturers of paper-based copper-coated board copper foil glue
Method.
Background technology
Paper-based copper-coated board manufacture roughening copper foil used, with one layer of copper foil glue must be first applied before prepreg hot pressing cladding
Glutinous agent, to meet the resistance to dip solderability requirement with peel strength of copper-clad plate product.Adhesive can also avoid making wiring board simultaneously
When copper foil is etched after paper fiber it is exposed in the environment, increase water absorption rate, reduce insulation resistance, cause circuit board to fail.Therefore,
Copper foil gluing agent prescription and its manufacturing process are the important components of paper-based copper-coated board production technology.Copper-clad plate production copper foil
Develop to slimming direction, traditional paper-based copper-coated board copper foil is based on 35um thickness, and 18um thickness copper foil has accounted for master at present
Lead status.15um, 13um thickness copper foil increase year by year in the use ratio of paper-based copper-coated board in recent years.With subtracting for copper thickness
Few, the roughening layer thickness of adhesive surface is also being reduced, and the peel strength of product is affected, and in electronic product assembling process, is held
Copper sheet obscission easily occurs, causes product rejection, economic loss serious.How to improve thin copper foil or extra thin copper foil paper substrate covers copper
The peel strength of plate improves the reliability of electronic product, is paper-based copper-coated board production firm concern.
Invention content
The purpose of the present invention is to provide a kind of paper-based copper-coated board manufacturing method of copper foil glue, copper foil glue obtained is apparent
The peel strength of copper-clad plate and the uniformity of peel strength are improved, in the production of slim copper foil paper-based copper-coated board, achieving
Preferable economic benefit.
In order to achieve the above objectives, solution of the invention is:
A kind of paper-based copper-coated board manufacturing method of copper foil glue, its step are as follows:
Step 1: the synthesis of modified ba phenolic resin
1) in 2350-2450 parts of phenol of addition, 3000-3200 parts of formaldehyde and 120-140 parts of trimerization in reaction kettle
Cyanamide formaldehyde resin is added 25-28 parts of barium hydroxide, carries out temperature reaction later in the case of stirring;
2) decompression dehydration after reaction, is vacuumized, 380-2300 parts of solvent is added after the completion, stirring later is simultaneously cold
But, deposit is for use;
Step 2: by the modification ba phenolic resin of obtained 240-260 parts and 150-160 parts of polyvinyl alcohol contracting fourth
Aldehyde, 18-22 parts of base epoxy resin mixed dissolution in 1090-1310 parts of organic solvent, you can copper foil of the present invention is made
Glue;
Described part is parts by weight.
The 1 of the step 1) in carry out temperature reaction, from beginning to warm to 80 DEG C, the time is 15 ± 5 minutes;Work as temperature
Nature heating, calculating reacting time when being warming up to 90 DEG C are carried out when rising to 80 DEG C, the reaction time is 60 minutes, keeps temperature 100
℃。
The 2 of the step 1) in, reaction terminates decompression dehydration immediately, and vacuum degree reaches 0.03Mpa in 5 minutes, final true
Reciprocal of duty cycle is 0.08-0.09 (5-10 points) Mpa;The big heating of steam when temperature is down to 70 DEG C, vapour pressure are less than 0.5Mpa;Dehydration temperaturre
When ging up to 75 DEG C, gel time is surveyed in sampling, is reached 90-110 seconds (160 DEG C), and stopping vacuumizes and is added 380-2300 parts
Solvent.
The 2 of the step 1) in, solvent is 380-400 parts of ethyl acetate and 1700-1900 parts of methanol.
In the step 2, first 1090-1310 parts of organic solvent is added in dissolving tank, is added in the case of stirring
150-160 parts of polyvinyl butyral, stirring and dissolving is until being completely dissolved;240-260 parts of modification barium is added later
Phenolic resin and 18-22 parts of base epoxy resin continue stirring and dissolving, obtain copper foil glue of the present invention.
In the step 2, organic solvent is 1000-1200 parts of methanol and 90-110 parts of acetone.
After adopting the above scheme, a kind of manufacturing method of paper-based copper-coated board copper foil glue of the present invention, has synthesized a kind of trimerization
Cyanamide formaldehyde resin is modified ba phenolic resin, and modified ba phenolic resin and polyvinyl butyral, base epoxy resin are existed
Copper foil glue is made in mixed dissolution in organic solvent, can significantly improve the peel strength of copper-clad plate and the uniformity of peel strength.
By the cyanurotriamide modified ba phenolic resin obtained by preparation method of the present invention, due to introducing stable heterocycle
The crosslink density of structure and resin improves, and the heat resistance of resin is remarkably improved, as the heat decomposition temperature of phenolic resin is
380 DEG C, be 438 DEG C after cyanurotriamide modified.In electronic product assembling process, it is not easy to which appearance layering, blistering, copper foil fall off
The defects of.In addition, cyanurotriamide modified ba phenolic resin, system polar groups increase, due to metal or metal oxide
Surface is all high energy surface, and highly polar adhesive is easy spreading wetting to copper foil surface, improves adhesion strength, improves copper foil
Peel strength, and improve the uniformity of peel strength.In being produced for slim copper foil paper-based copper-coated board, preferable economy is achieved
Benefit.
Specific implementation mode
The present invention will be further described in detail with reference to the specific embodiments.
The present invention relates to a kind of paper-based copper-coated board manufacturing methods of copper foil glue, and its step are as follows:
Step 1: the synthesis of modified ba phenolic resin
1) in 2350-2450 parts of phenol of addition, 3000-3200 parts of formaldehyde and 120-140 parts of trimerization in reaction kettle
Cyanamide formaldehyde resin is added 25-28 parts of barium hydroxide, carries out temperature reaction later in the case of stirring;
The phenol, formaldehyde and melamine resin are sequentially added into reaction kettle and stir, the case where stirring
Lower addition barium hydroxide, stirring start to warm up reaction in 3-5 minutes;
The temperature reaction, concrete operations embodiment are that, from beginning to warm to 80 DEG C, the time is 15 ± 5 minutes;Work as temperature
When rising to 80 DEG C, closing porthole makes it heat up naturally, calculating reacting time when being warming up to 90 DEG C, and the reaction time is 60 minutes, is protected
Hold 100 DEG C of temperature.
2) decompression dehydration after reaction, is vacuumized, 380-2300 parts of solvent is added after the completion, stirring later is simultaneously cold
But, deposit is for use;One preferred embodiment of the solvent is 380-400 parts of ethyl acetate and 1700-1900 parts of methanol.
It is to reach 0.03Mpa in vacuum degree in 5 minutes that the reaction, which terminates decompression dehydration, concrete operations embodiment immediately,
Final vacuum degree is 0.08-0.09 (5-10 points) Mpa;The big heating of steam is opened 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, is reached 90-110 seconds (160 DEG C), and stopping vacuumizes and 380- is added
2300 parts of solvent;Solvent stirs after being added, and is cooled to 40 DEG C, and it is for use to stop stirring deposit.
Shown in the synthetic material and proportioning table specific as follows of the modified ba phenolic resin.
Serial number | Raw material title | Specification | Inventory (kg) |
1 | Phenol | Industrial level-one | 2350-2450 |
2 | Formaldehyde | 37% | 3000-3200 |
3 | Melamine resin | 45% | 120-140 |
4 | Barium hydroxide | C.P | 25-28 |
5 | Ethyl acetate | It is qualified | 380-400 |
6 | Methanol | It is qualified | 1700-1900 |
For the synthetic material and proportioning of modified ba phenolic resin, provide shown in the following table of a specific embodiment.
Serial number | Raw material title | Specification | Inventory (kg) |
1 | Phenol | Industrial level-one | 2400 |
2 | Formaldehyde | 37% | 3150 |
3 | Melamine resin | 45% | 120 |
4 | Barium hydroxide | C.P | 27 |
5 | Ethyl acetate | It is qualified | 396 |
6 | Methanol | It is qualified | 1800 |
Synthesized modified ba phenolic resin obtained, quality index is with reference to shown in lower table.
Detection project | Testing conditions | Examination criteria |
Appearance | Room temperature | Brownish red transparency liquid |
Gel time | 160±2℃ | 60-80 seconds |
Solid content | 140℃ 1H | 52-56% |
Step 2: by the modification ba phenolic resin of obtained 240-260 parts and 150-160 parts of polyvinyl alcohol contracting fourth
Aldehyde, 18-22 parts of base epoxy resin mixed dissolution in 1090-1310 parts of organic solvent, you can copper foil of the present invention is made
Glue.The organic solvent preferred embodiment is 1000-1200 parts of methanol and 90-110 parts of acetone.
Dissolving operating procedure preferred embodiment is that first 1090-1310 parts of organic solvent is added and (first is successively added in order
Alcohol and acetone) in dissolving tank, 150-160 parts of polyvinyl butyral is added in the case of stirring, stirring and dissolving is until complete
Until fully dissolved, the stirring and dissolving time is preferably no fewer than 8 hours;Later be added 240-260 part modification ba phenolic resin with
18-22 parts of base epoxy resin continues stirring and dissolving (dissolving 1 hour), later releases glue, sampling and testing, meet mark
Standard obtains copper foil glue of the present invention and uses.
Above-described part is parts by weight.
Shown in the raw material and the following table of proportioning that the copper foil glue is prepared.
Serial number | Raw material title | Specification | Inventory (kg) |
1 | Methanol | It is qualified | 1000-1200 |
2 | Acetone | It is qualified | 90-110 |
3 | Polyvinyl butyral | It is qualified | 150-160 |
4 | Modified ba phenolic resin | 50% | 240-260 |
5 | Base epoxy resin | It is qualified | 18-22 |
The raw material and proportioning prepared for copper foil glue, provide shown in the following table of a specific embodiment.
Serial number | Raw material title | Specification | Inventory (kg) |
1 | Methanol | It is qualified | 1150 |
2 | Acetone | It is qualified | 100 |
3 | Polyvinyl butyral | It is qualified | 150 |
4 | Modified ba phenolic resin | 50% | 250 |
5 | Base epoxy resin | It is qualified | 20 |
Synthesized copper foil glue obtained, quality index is with reference to shown in lower table.
Serial number | Project name | Standard |
1 | Appearance | Yellow or amber transparent liquid |
2 | Solid content (150 DEG C, 1 hour) | 17-20% |
Copper foil glue application example produced by the present invention is as follows:The above prepared copper foil glue is coated in 15um or 12um thickness
On the roughening copper foil of degree, through drying and removing solvent at 140-16 DEG C, and acetone soluble 20-30% is controlled, glue-spread is often put down
Square rice 14g-16g, is made adhesive coated foil.It is overlapped with 1 adhesive coated foil and 8 paper substrate prepregs, in 100Kg/cm2, 160 DEG C
Under the conditions of hot pressing 100 minutes, that is, the copper-clad laminate that thickness is 1.6mm is made.Plank resistance to dip solderability (260 DEG C) 15 seconds with
On, peel strength 1.2-1.4N/mm, other performances reach CPFCP-04 technical requirements in GB 4723-92 standards.
The foregoing is merely the preferred embodiment of the present invention, all equivalent changes done with scope of the invention as claimed and
Modification, should all belong to the range of the claims in the present invention.
Claims (6)
1. a kind of paper-based copper-coated board manufacturing method of copper foil glue, which is characterized in that steps are as follows:
Step 1: the synthesis of modified ba phenolic resin
1) in 2350-2450 parts of phenol of addition, 3000-3200 parts of formaldehyde and 120-140 parts of melamine in reaction kettle
Formaldehyde resin is added 25-28 parts of barium hydroxide, carries out temperature reaction later in the case of stirring;
2) decompression dehydration after reaction, is vacuumized, 380-2300 parts of solvent is added after the completion, is stirred later and cooling, storage
It is standby for use;
Step 2: polyvinyl butyral, 18- by the modification ba phenolic resin of obtained 240-260 parts with 150-160 parts
22 parts of base epoxy resin mixed dissolution in 1090-1310 parts of organic solvent, you can the copper foil glue is made;
Described part is parts by weight.
2. a kind of manufacturing method of paper-based copper-coated board copper foil glue as described in claim 1, which is characterized in that the step 1
1) in carry out temperature reaction, from beginning to warm to 80 DEG C, the time is 15 ± 5 minutes;Nature is carried out when temperature rises to 80 DEG C
Heating, calculating reacting time when being warming up to 90 DEG C, reaction time are 60 minutes, keep 100 DEG C of temperature.
3. a kind of manufacturing method of paper-based copper-coated board copper foil glue as described in claim 1, which is characterized in that the step 1
2) in, reaction terminates decompression dehydration immediately, and vacuum degree reaches 0.03Mpa in 5 minutes, finally the vacuum in 5-10 minutes
Degree reaches 0.08-0.09Mpa;The big heating of steam when temperature is down to 70 DEG C, vapour pressure are less than 0.5Mpa;Dehydration temperaturre is gone up to 75
DEG C when, sample simultaneously survey gel time under the conditions of 160 degree, reach 90-110 seconds, stop vacuumize and be added 380-2300 parts
Solvent.
4. a kind of manufacturing method of paper-based copper-coated board copper foil glue as described in claim 1 or 3, which is characterized in that the step
The 2 of rapid one) in, solvent is 380-400 parts of ethyl acetate and 1700-1900 parts of methanol.
5. a kind of manufacturing method of paper-based copper-coated board copper foil glue as described in claim 1, which is characterized in that the step 2
In, first 1090-1310 parts of organic solvent is added in dissolving tank, 150-160 parts of polyethylene is added in the case of stirring
Butyral, stirring and dissolving is until being completely dissolved;Later be added 240-260 parts modification ba phenolic resin and 18-22 parts
Base epoxy resin, continue stirring and dissolving, obtain the copper foil glue.
6. a kind of manufacturing method of paper-based copper-coated board copper foil glue as described in claim 1 or 5, which is characterized in that the step
In rapid two, organic solvent is 1000-1200 parts of methanol and 90-110 parts of acetone.
Priority Applications (3)
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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 |
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CN201510951816.7A CN105542692B (en) | 2015-12-17 | 2015-12-17 | A kind of manufacturing method of paper-based copper-coated board copper foil glue |
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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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CN105542692B true 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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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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CN113388349B (en) * | 2021-05-13 | 2023-03-31 | 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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Publication number | Publication date |
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CN108977144B (en) | 2021-01-08 |
CN108977144A (en) | 2018-12-11 |
CN109082252A (en) | 2018-12-25 |
CN105542692A (en) | 2016-05-04 |
CN109082252B (en) | 2021-01-08 |
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