CN107488331A - Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof for paper-based copper-coated board - Google Patents
Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof for paper-based copper-coated board Download PDFInfo
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- CN107488331A CN107488331A CN201710707068.7A CN201710707068A CN107488331A CN 107488331 A CN107488331 A CN 107488331A CN 201710707068 A CN201710707068 A CN 201710707068A CN 107488331 A CN107488331 A CN 107488331A
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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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
- C08G8/32—Chemically modified polycondensates by organic acids or derivatives thereof, e.g. fatty oils
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08L2201/02—Flame or fire retardant/resistant
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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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Abstract
The invention discloses a kind of epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof for paper-based copper-coated board, comprise the following steps:After epoxidized soybean oil epoxy ring-opening, addition is carried out with the phenolic hydroxyl group on bisphenol-A and anacardol, obtains addition product A;After addition product A and phenol, formaldehyde reaction, gel, epoxy soybean oil-modified resin B then is made through vacuum dehydration;Tung oil is added in epoxy soybean oil-modified resin B, epoxy resin and fire retardant are added after stirring, continues to be uniformly mixed and produces.Present invention reduces dependence of the large-scale production copper-clad plate to tung oil, the tung oil production pressure in short supply brought is alleviated, and epoxidized soybean oil market is wide, it is cheap, reduce production cost, it is gained glue anti-flammability, heat-resist, using wide, bonding force is strong, and cost is low, safety and environmental protection, production for paper-based copper-coated board, with low manufacture cost, product quality is stable, meets JISC6485 standard requirement.
Description
Technical field
The present invention relates to printed-board technology field, more particularly to a kind of epoxidized soybean oil for paper-based copper-coated board to change
Property phenolic resin glue liquid and preparation method thereof.
Background technology
Copper-clad plate is the important materials of printed circuit board industry, and paper-based copper-coated board is one of copper-clad plate principal item, largely
For domestic electronic appliances such as TVs.The manufacturing process of paper-based copper-coated board uses tung oil modified phenolic resin more, then in wood pulp
It is impregnated with, dries on paper, after obtaining prepreg, overlapping is compounded in progress hot pressing with copper foil and produced.During its production and use,
Security reliability is the major criterion of product.Phenolic resin be at first find and first industrialized production a kind of synthetic resin, but
It is that the paper-based copper-coated board prepared using phenol-formaldehyde resin modified at present is more to be modified phenolic resin with tung oil.However, due to paulownia
Oily market price fluctuations are larger, in short supply, do not only result in the paper-based copper-coated board material cost of raw material rise it is larger, and to big rule
Mould production brings very big pressure.Therefore, the replacement part tung oil of modified oils turns into a kind of new development trend.Based on above-mentioned old
State, the present invention proposes a kind of epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof for paper-based copper-coated board.
The content of the invention
The invention aims to solve shortcoming present in prior art, and the one kind proposed is used for paper-based copper-coated board
Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof.
For the epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof of paper-based copper-coated board, comprise the following steps:
S1, preparation prepare the raw material of epoxidized soybean oil modified alkyd resin glue liquid, including epoxidized soybean oil, bisphenol-A, anacardol,
Phenol, formaldehyde, tung oil, epoxy resin, fire retardant
S2, by after epoxidized soybean oil epoxy ring-opening, carry out addition with the phenolic hydroxyl group on bisphenol-A and anacardol, obtain addition product A;
S3, by addition product A in the basic conditions, 2.2~2.8h is reacted under conditions of 85~102 DEG C with phenol, formaldehyde, complete
After phenolic aldehyde polycondensation reaction, under conditions of 168~185 DEG C, 2~6min of gel, epoxidized soybean oil then is made through vacuum dehydration
Modified resin B;
S4, tung oil is added in step S3 in the epoxy soybean oil-modified resin B of gained, with 280~420r/min rotating speed
After stirring 10~20min, epoxy resin and fire retardant are added, continues to be stirred 30~50min, it is well mixed to produce required ring
The soybean oil modified phenolic resin glue of oxygen.
Preferably, the mass ratio of epoxidized soybean oil, bisphenol-A and anacardol is 2~5 in the step S2:1~2.2:1~
2.2。
Preferably, the alkalescence condition in the step S3 is that pH value is 7.8~11.4.
Preferably, the mass ratio of the addition product A in the step S3, phenol and formaldehyde is 1.8~3:1.5~2:1~
1.2。
Preferably, the addition of tung oil is the 0.35~0.48 of epoxy soybean oil-modified resin B total amounts in the step S4
Times;The addition of epoxy resin is 1.2~1.8 times of epoxy soybean oil-modified resin B total amounts;The addition of fire retardant is epoxy
0.1~0.3 times of soybean oil modified resin B total amount.
Preferably, the fire retardant in the step S4 is that mass ratio is 2~3:1.5~1.8:0.5~1.1 hydroxide
The composition of aluminium, magnesium hydroxide and microcapsule red phosphorus.
Preferably, in the step S4 obtained epoxidized soybean oil modified alkyd resin glue liquid can coordinate it is cyanurotriamide modified
Linear phenolic resin, semi-finished product gummed paper is made using secondary photoresist coating process, finally by semi-finished product gummed paper and copper foil it is compound after heat
Press and produce paper-based copper-coated board.
A kind of epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof for paper-based copper-coated board proposed by the present invention, is adopted
After epoxy soybean oil-modified resin, after epoxy soybean oil-modified resin is rationally mixed with tung oil, epoxy resin and fire retardant
Epoxidized soybean oil modified alkyd resin glue liquid of the institute required to paper-based copper-coated board is made, preparation method proposed by the present invention operation is simple
It is single, prepare that cost is low, it effectively reduces dependence of the large-scale production copper-clad plate to tung oil, alleviates that tung oil is in short supply to be brought
Production pressure, and epoxidized soybean oil market is wide, cheap, considerably reduces production cost, gained glue has fire-retardant
Property, heat-resist, use is wide, and bonding force is strong, and cost is low, the advantage such as safety and environmental protection, for the production of paper-based copper-coated board, has
Low manufacture cost, product quality is stable, meets JISC6485 standard requirement.
Embodiment
The present invention is made with reference to specific embodiment further to explain.
Embodiment one
Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof proposed by the present invention for paper-based copper-coated board, including following step
Suddenly:
S1, preparation prepare the raw material of epoxidized soybean oil modified alkyd resin glue liquid, including epoxidized soybean oil, bisphenol-A, anacardol,
Phenol, formaldehyde, tung oil, epoxy resin, fire retardant
S2, in mass ratio 4.2:2:1.8, after epoxidized soybean oil epoxy ring-opening, with the phenolic hydroxyl group on bisphenol-A and anacardol
Addition is carried out, obtains addition product A;
S3, in mass ratio 2.6:2:1.1, by addition product A in the case where pH value is 11 alkalescence condition, with phenol, formaldehyde at 98 DEG C
Under the conditions of react 2.5h, after completing phenolic aldehyde polycondensation reaction, under conditions of 180 DEG C, gel 5min, be then made through vacuum dehydration
Epoxy soybean oil-modified resin B;
S4, by 0.45 times of tung oil epoxy soybean oil-modified resin B total amounts of the epoxidized soybean oil for being added in step S3 gained
In modified resin B, after 400r/min rotating speed stirring 18min, 1.6 times of epoxy soybean oil-modified resin B total amounts are added
Epoxy resin and 0.3 times of mass ratio of epoxy soybean oil-modified resin B total amounts are 2.8:1.7:1 aluminium hydroxide, hydroxide
The composition of magnesium and microcapsule red phosphorus, continue to be stirred 45min, it is well mixed to produce required epoxidized soybean oil modified phenolic resin
Fat glue.
Embodiment two
Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof proposed by the present invention for paper-based copper-coated board, including following step
Suddenly:
S1, preparation prepare the raw material of epoxidized soybean oil modified alkyd resin glue liquid, including epoxidized soybean oil, bisphenol-A, anacardol,
Phenol, formaldehyde, tung oil, epoxy resin, fire retardant
S2, in mass ratio 2:1:1, after epoxidized soybean oil epoxy ring-opening, carried out with the phenolic hydroxyl group on bisphenol-A and anacardol
Addition, obtain addition product A;
S3, in mass ratio 1.8:1.5:1, by addition product A in the case where pH value is 7.8 alkalescence condition, with phenol, formaldehyde at 85 DEG C
Under the conditions of react 2.2h, after completing phenolic aldehyde polycondensation reaction, under conditions of 168 DEG C, gel 2min, be then made through vacuum dehydration
Epoxy soybean oil-modified resin B;
S4, by 0.35 times of tung oil epoxy soybean oil-modified resin B total amounts of the epoxidized soybean oil for being added in step S3 gained
In modified resin B, after 280r/min rotating speed stirring 10min, 1.2 times of epoxy soybean oil-modified resin B total amounts are added
Epoxy resin and 0.1 times of mass ratio of epoxy soybean oil-modified resin B total amounts are 2:1.5:0.5 aluminium hydroxide, hydroxide
The composition of magnesium and microcapsule red phosphorus, continue to be stirred 30min, it is well mixed to produce required epoxidized soybean oil modified phenolic resin
Fat glue.
Embodiment three
Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof proposed by the present invention for paper-based copper-coated board, including following step
Suddenly:
S1, preparation prepare the raw material of epoxidized soybean oil modified alkyd resin glue liquid, including epoxidized soybean oil, bisphenol-A, anacardol,
Phenol, formaldehyde, tung oil, epoxy resin, fire retardant
S2, in mass ratio 3.5:1.6:1.8, after epoxidized soybean oil epoxy ring-opening, with the phenol hydroxyl on bisphenol-A and anacardol
Base carries out addition, obtains addition product A;
S3, in mass ratio 2.4:1.8:1.2, by addition product A in the case where pH value is 10.2 alkalescence condition, with phenol, formaldehyde 94
2.5h is reacted under conditions of DEG C, after completing phenolic aldehyde polycondensation reaction, under conditions of 176 DEG C, gel 4min, then through vacuum dehydration
Epoxy soybean oil-modified resin B is made;
S4, by 0.42 times of tung oil epoxy soybean oil-modified resin B total amounts of the epoxidized soybean oil for being added in step S3 gained
In modified resin B, after 350r/min rotating speed stirring 15min, 1.5 times of epoxy soybean oil-modified resin B total amounts are added
Epoxy resin and 0.2 times of mass ratio of epoxy soybean oil-modified resin B total amounts are 2.5:1.7:0.8 aluminium hydroxide, hydrogen-oxygen
Change the composition of magnesium and microcapsule red phosphorus, continue to be stirred 40min, it is well mixed to produce required epoxidized soybean oil modified phenolic
Resin adhesive liquid.
Example IV
Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof proposed by the present invention for paper-based copper-coated board, including following step
Suddenly:
S1, preparation prepare the raw material of epoxidized soybean oil modified alkyd resin glue liquid, including epoxidized soybean oil, bisphenol-A, anacardol,
Phenol, formaldehyde, tung oil, epoxy resin, fire retardant
S2, in mass ratio 5:2.2:2, after epoxidized soybean oil epoxy ring-opening, enter with the phenolic hydroxyl group on bisphenol-A and anacardol
Row addition, obtain addition product A;
S3, in mass ratio 3:2:1.2, by addition product A in the case where pH value is 11.4 alkalescence condition, with phenol, formaldehyde at 102 DEG C
Under the conditions of react 2.8h, after completing phenolic aldehyde polycondensation reaction, under conditions of 185 DEG C, gel 6min, be then made through vacuum dehydration
Epoxy soybean oil-modified resin B;
S4, by 0.48 times of tung oil epoxy soybean oil-modified resin B total amounts of the epoxidized soybean oil for being added in step S3 gained
In modified resin B, after 420r/min rotating speed stirring 20min, 1.8 times of epoxy soybean oil-modified resin B total amounts are added
Epoxy resin and 0.3 times of mass ratio of epoxy soybean oil-modified resin B total amounts are 3:1.8:1.1 aluminium hydroxide, hydroxide
The composition of magnesium and microcapsule red phosphorus, continue to be stirred 50min, it is well mixed to produce required epoxidized soybean oil modified phenolic resin
Fat glue.
Embodiment five
Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof proposed by the present invention for paper-based copper-coated board, including following step
Suddenly:
S1, preparation prepare the raw material of epoxidized soybean oil modified alkyd resin glue liquid, including epoxidized soybean oil, bisphenol-A, anacardol,
Phenol, formaldehyde, tung oil, epoxy resin, fire retardant
S2, in mass ratio 2.5:1.2:1, after epoxidized soybean oil epoxy ring-opening, with the phenolic hydroxyl group on bisphenol-A and anacardol
Addition is carried out, obtains addition product A;
S3, in mass ratio 2:1.6:1.1, by addition product A in the case where pH value is 8.4 alkalescence condition, with phenol, formaldehyde 85~
2.4h is reacted under conditions of 102 DEG C, after completing phenolic aldehyde polycondensation reaction, under conditions of 174 DEG C, gel 3min, then through vacuum
Epoxy soybean oil-modified resin B is made in dehydration;
S4, by 0.38 times of tung oil epoxy soybean oil-modified resin B total amounts of the epoxidized soybean oil for being added in step S3 gained
In modified resin B, after 300r/min rotating speed stirring 12min, 1.4 times of epoxy soybean oil-modified resin B total amounts are added
Epoxy resin and 0.15 times of mass ratio of epoxy soybean oil-modified resin B total amounts are 2.2:1.6:0.8 aluminium hydroxide, hydrogen-oxygen
Change the composition of magnesium and microcapsule red phosphorus, continue to be stirred 35min, it is well mixed to produce required epoxidized soybean oil modified phenolic
Resin adhesive liquid.
The epoxidized soybean oil modified alkyd resin glue liquid for paper-based copper-coated board prepared in the embodiment of the present invention one is matched somebody with somebody
Cyanurotriamide modified linear phenolic resin is closed, semi-finished product gummed paper is made using secondary photoresist coating process, finally by semi-finished product gummed paper
Paper-based copper-coated board is produced with the compound rear hot pressing of copper foil, the paper-based copper-coated board performance indications of preparation is tested, draws following parameter:
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, it is any
Those familiar with the art the invention discloses technical scope in, technique according to the invention scheme and its invention
Design is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (7)
1. the epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof for paper-based copper-coated board, it is characterised in that including following
Step:
S1, preparation prepare the raw material of epoxidized soybean oil modified alkyd resin glue liquid, including epoxidized soybean oil, bisphenol-A, anacardol,
Phenol, formaldehyde, tung oil, epoxy resin, fire retardant
S2, by after epoxidized soybean oil epoxy ring-opening, carry out addition with the phenolic hydroxyl group on bisphenol-A and anacardol, obtain addition product A;
S3, by addition product A in the basic conditions, 2.2~2.8h is reacted under conditions of 85~102 DEG C with phenol, formaldehyde, complete
After phenolic aldehyde polycondensation reaction, under conditions of 168~185 DEG C, 2~6min of gel, epoxidized soybean oil then is made through vacuum dehydration
Modified resin B;
S4, tung oil is added in step S3 in the epoxy soybean oil-modified resin B of gained, with 280~420r/min rotating speed
After stirring 10~20min, epoxy resin and fire retardant are added, continues to be stirred 30~50min, it is well mixed to produce required ring
The soybean oil modified phenolic resin glue of oxygen.
2. the epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof according to claim 1 for paper-based copper-coated board,
Characterized in that, the mass ratio of epoxidized soybean oil, bisphenol-A and anacardol is 2~5 in the step S2:1~2.2:1~2.2.
3. the epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof according to claim 1 for paper-based copper-coated board,
Characterized in that, it is 7.8~11.4 that the alkalescence condition in the step S3, which is pH value,.
4. the epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof according to claim 1 for paper-based copper-coated board,
Characterized in that, the mass ratio of the addition product A, phenol and formaldehyde in the step S3 are 1.8~3:1.5~2:1~1.2.
5. the epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof according to claim 1 for paper-based copper-coated board,
Characterized in that, the addition of tung oil is 0.35~0.48 times of epoxy soybean oil-modified resin B total amounts in the step S4;Ring
The addition of oxygen tree fat is 1.2~1.8 times of epoxy soybean oil-modified resin B total amounts;The addition of fire retardant is epoxy soybean
0.1~0.3 times of oil-modified resin B total amounts.
6. the epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof according to claim 1 for paper-based copper-coated board,
Characterized in that, it is 2~3 that the fire retardant in the step S4, which is mass ratio,:1.5~1.8:0.5~1.1 aluminium hydroxide, hydrogen
The composition of magnesia and microcapsule red phosphorus.
7. the epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof according to claim 1 for paper-based copper-coated board,
Characterized in that, obtained epoxidized soybean oil modified alkyd resin glue liquid can coordinate cyanurotriamide modified line in the step S4
Property phenolic resin, semi-finished product gummed paper is made using secondary photoresist coating process, finally by semi-finished product gummed paper and copper foil it is compound after hot pressing be
Obtain paper-based copper-coated board.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107955328A (en) * | 2017-12-27 | 2018-04-24 | 珠海邦瑞合成材料有限公司 | A kind of low-temperature fast-curing thermoplasticity powder phenolic resin for color resin grinding tool and preparation method thereof |
CN113061223A (en) * | 2021-03-23 | 2021-07-02 | 建滔(佛冈)积层纸板有限公司 | Preparation method of epoxy soybean oil modified resin and method for preparing paper-based copper-clad plate |
CN113088032A (en) * | 2021-03-25 | 2021-07-09 | 建滔(佛冈)积层纸板有限公司 | Linear phenolic resin and method for manufacturing high-performance halogen-free environment-friendly paper-based copper-clad plate by using same |
CN115286900A (en) * | 2022-09-06 | 2022-11-04 | 陕西生益科技有限公司 | Resin composition and application thereof |
-
2017
- 2017-08-17 CN CN201710707068.7A patent/CN107488331A/en not_active Withdrawn
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107955328A (en) * | 2017-12-27 | 2018-04-24 | 珠海邦瑞合成材料有限公司 | A kind of low-temperature fast-curing thermoplasticity powder phenolic resin for color resin grinding tool and preparation method thereof |
CN113061223A (en) * | 2021-03-23 | 2021-07-02 | 建滔(佛冈)积层纸板有限公司 | Preparation method of epoxy soybean oil modified resin and method for preparing paper-based copper-clad plate |
CN113061223B (en) * | 2021-03-23 | 2022-04-08 | 建滔(佛冈)积层纸板有限公司 | Preparation method of epoxy soybean oil modified resin and method for preparing paper-based copper-clad plate |
CN113088032A (en) * | 2021-03-25 | 2021-07-09 | 建滔(佛冈)积层纸板有限公司 | Linear phenolic resin and method for manufacturing high-performance halogen-free environment-friendly paper-based copper-clad plate by using same |
CN115286900A (en) * | 2022-09-06 | 2022-11-04 | 陕西生益科技有限公司 | Resin composition and application thereof |
CN115286900B (en) * | 2022-09-06 | 2023-11-10 | 陕西生益科技有限公司 | Resin composition and application thereof |
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