JPS62295929A - Preparation of resin-impregnated base material - Google Patents
Preparation of resin-impregnated base materialInfo
- Publication number
- JPS62295929A JPS62295929A JP13898186A JP13898186A JPS62295929A JP S62295929 A JPS62295929 A JP S62295929A JP 13898186 A JP13898186 A JP 13898186A JP 13898186 A JP13898186 A JP 13898186A JP S62295929 A JPS62295929 A JP S62295929A
- Authority
- JP
- Japan
- Prior art keywords
- base material
- resin
- impregnated
- weight
- paper
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 69
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Inorganic materials O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229920005989 resin Polymers 0.000 claims abstract description 46
- 239000011347 resin Substances 0.000 claims abstract description 46
- 239000002966 varnish Substances 0.000 claims abstract description 44
- 239000005011 phenolic resin Substances 0.000 claims abstract description 19
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 150000002366 halogen compounds Chemical class 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000000123 paper Substances 0.000 abstract description 48
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000003822 epoxy resin Substances 0.000 abstract description 4
- 229910052736 halogen Inorganic materials 0.000 abstract description 4
- 150000002367 halogens Chemical class 0.000 abstract description 4
- 229920000647 polyepoxide Polymers 0.000 abstract description 4
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002655 kraft paper Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 description 18
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 15
- 239000003063 flame retardant Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 229920003987 resole Polymers 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- FVCSARBUZVPSQF-UHFFFAOYSA-N 5-(2,4-dioxooxolan-3-yl)-7-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C(C(OC2=O)=O)C2C(C)=CC1C1C(=O)COC1=O FVCSARBUZVPSQF-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- QEZIKGQWAWNWIR-UHFFFAOYSA-N antimony(3+) antimony(5+) oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[Sb+3].[Sb+5] QEZIKGQWAWNWIR-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- -1 nitrogen-containing compound Chemical class 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 239000011134 resol-type phenolic resin Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000002383 tung oil Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0366—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement reinforced, e.g. by fibres, fabrics
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
Landscapes
- Reinforced Plastic Materials (AREA)
- Laminated Bodies (AREA)
Abstract
Description
【発明の詳細な説明】
３、発明の詳細な説明
［技術分野］
本発明は、印刷回路用銅張積層板などの製造に用いられ
る樹脂含浸基材の製造方法に関するものである。Detailed Description of the Invention 3. Detailed Description of the Invention [Technical Field] The present invention relates to a method for manufacturing a resin-impregnated base material used for manufacturing copper-clad laminates for printed circuits and the like.
［背景技術］
印刷回路用銅張積層板は所要枚数の樹脂含浸基材を重ね
、さらにこれに銅箔などの金属箔を重ねて加熱加圧する
ことによって作成される。そして印刷回路用鋼張積層板
の難燃性を高めるためには樹脂含浸基材の難燃化を進め
る必要がある。そして樹脂含浸基材の難燃化のために従
来から種々の方法が採用されており、次にその代表的な
ものを列挙する。[Background Art] Copper-clad laminates for printed circuits are produced by stacking a required number of resin-impregnated base materials, and then stacking metal foil such as copper foil on top of this and heating and pressurizing the stack. In order to improve the flame retardancy of steel-clad laminates for printed circuits, it is necessary to make the resin-impregnated base material flame retardant. Various methods have heretofore been employed to make resin-impregnated base materials flame retardant, and representative methods are listed below.
■ 含浸樹脂にテトラブロムビスフェノールＡなどのハ
ロゲンやリンを含む難燃剤を添加する方法■ 基材をメ
ラミン等の含窒素化合物で処理する方法
■ 上記の■と■の方法を併用する方法■ 三酸化アン
チモンとハロゲン化合物とを併用して樹脂とともに基材
に含浸させろ方法しかし■の方法では、十分な難燃効果
を得るためには多量のハロゲンやリンを含む難燃剤が必
要であって製造コストが高くなり、しかもこの難燃剤の
多量配合によって耐熱性が低下するという問題があり、
■の方法では十分な難燃効果が得られず、■の方法では
■の場合と同様に耐熱性が低下するという問題ある。さ
らに■の方法ではワニス中で三酸化アンチモンが沈降し
易くて基材に二酸化アンチモンを均一に分散させること
が難しく、このために作業性が悪いと共に安定した難燃
性を得ることが難しいという問題がある。■ A method of adding a flame retardant containing halogen or phosphorus such as tetrabromo bisphenol A to the impregnating resin ■ A method of treating the base material with a nitrogen-containing compound such as melamine ■ A method of combining the above methods ■ and ■ ■ Trioxide Method of impregnating a base material with a resin using a combination of antimony and a halogen compound However, in method (2), in order to obtain a sufficient flame retardant effect, a large amount of flame retardant containing halogen and phosphorus is required, resulting in high production costs. Moreover, there is a problem that the heat resistance decreases due to the large amount of flame retardant added.
Method (2) does not provide a sufficient flame retardant effect, and method (2) has the same problem as the method (2) in that the heat resistance decreases. Furthermore, in method (2), antimony trioxide tends to settle in the varnish, making it difficult to uniformly disperse antimony dioxide in the base material, resulting in poor workability and difficulty in achieving stable flame retardancy. There is.
［発明の目的］
本発明は、上記の点に鑑みて為されたものであり、耐熱
性を低下させることなく安定した＠燃性を得ることがで
きる樹脂含浸基材の製造方法を提供することを目的とす
るものである。[Object of the invention] The present invention has been made in view of the above points, and an object of the present invention is to provide a method for producing a resin-impregnated base material that can obtain stable @flammability without reducing heat resistance. The purpose is to
［発明の開示］
しかして本発明に係る樹脂含浸基材の製造方法は、五酸
化アンチモンが配合されたフェノール系樹脂ワニスを紙
基材に一次含浸させたのちに、ハロゲン化合物を含む樹
脂ワニスを紙基材に含浸させ、これを乾燥することを特
徴とするものであり、以下本発明の詳細な説明する。[Disclosure of the Invention] The method for producing a resin-impregnated base material according to the present invention involves first impregnating a paper base material with a phenolic resin varnish containing antimony pentoxide, and then applying a resin varnish containing a halogen compound. The present invention is characterized in that it is impregnated into a paper base material and then dried, and the present invention will be described in detail below.
前述の■〜■の方法は耐熱性等において問題が生じるた
めに、本発明では■の方法のようにハロゲン化合物を難
燃剤としアンチモンを難燃助剤として用いることによっ
て耐熱性を低下させるハロゲン化合物の使用量を低減で
きろようにするのであるが、この場合、アンチモンとし
て三酸化アンチモンを用いると前述のように分散性の問
題がある。そして本発明者等はアンチモンとして三酸化
アンチモンと同様にハロゲン化合物の難燃助剤とし、て
作■する五酸化アンチモン（Ｓ ｂ２０ 、・４Ｈ２０
）を用いた場合には、フェノール系樹脂ワニス中に均一
に分散させることができることを見出だして本発明を完
成したものである。一方、紙を基材とする樹脂含浸基材
の耐湿性を向上させるために、紙基材に水溶媒を含有す
る親水性の７二ノ一ルｉｋ！Ｍ脂を一次含浸として含浸
して乾燥したのちに、目的とする含浸樹脂をさらに紙基
材に含浸させる方法が一般におこなわれているが、この
ような水溶媒を含む親水性のフェノール系ム（脂ワニス
中で五酸化アンチモンは一層良好に分散し、しかも沈降
することなく安定して存在する。そこで本発明において
は五酸化アンチモンを水溶媒を含むフェノール系樹脂ワ
ニスに分散させてこれを紙基材に一次含浸として含浸さ
せるようにするのがよい。Since the above-mentioned methods (1) to (2) cause problems in heat resistance, etc., in the present invention, as in method (1), a halogen compound is used as a flame retardant and antimony is used as a flame retardant auxiliary agent to reduce heat resistance. However, in this case, if antimony trioxide is used as the antimony, there is a problem with dispersibility as described above. The present inventors used antimony pentoxide (S b20 , 4H20
), the present invention was completed by discovering that it can be uniformly dispersed in a phenolic resin varnish. On the other hand, in order to improve the moisture resistance of a paper-based resin-impregnated base material, a hydrophilic 72-no-1 ik! that contains a water solvent in the paper base material has been developed. Generally, the paper base material is impregnated with M resin as a primary impregnation and dried, and then the target impregnation resin is further impregnated into the paper base material. Antimony pentoxide is better dispersed in fatty varnish and exists stably without settling.Therefore, in the present invention, antimony pentoxide is dispersed in a phenolic resin varnish containing an aqueous solvent and then applied to a paper base. It is preferable to impregnate the material as a primary impregnation.
しかして、紙基材としてはクラフト紙やリンク−紙など
が用いられ、この紙基材に五酸化アンチモンを配合した
７エ／−ル系樹脂ワニスを一次含浸として含浸させて乾
燥する。このフェノール系樹脂ワニスはフェノール樹脂
あるいは変性フェノール樹脂を水にメタノール、トルエ
ン、アセトン、メチルエチルケトンなどの揮発性有機溶
媒を加えた混合溶媒に溶解することによって調製される
。As the paper base material, kraft paper, link paper, etc. are used, and this paper base material is impregnated with a 7-er resin varnish containing antimony pentoxide as a primary impregnation, and then dried. This phenolic resin varnish is prepared by dissolving a phenolic resin or a modified phenolic resin in a mixed solvent of water and a volatile organic solvent such as methanol, toluene, acetone, or methyl ethyl ketone.
水は紙基材に浸透し易く、従って紙基材へのフェノール
系樹脂の含浸を促す作用もなす。また有機溶媒はワニス
への７二７−ル系樹脂の溶解性を高めると共に紙基材に
フェノール系！Ｉ脂ワニスを含浸したのちの乾燥を速め
る作用をなす。また７ヱ／−ル系樹脂ワニスに難燃助剤
として配合される五酸化アンチモンが安定して存在する
ために、ワニスの溶媒中の２０重量％以上が水溶媒であ
ることが望ましい。Water easily penetrates into the paper base material, and therefore also acts to promote impregnation of the phenolic resin into the paper base material. In addition, organic solvents increase the solubility of 727-based resins in varnishes, and phenolics are used for paper base materials! It has the effect of speeding up drying after being impregnated with I-fat varnish. Furthermore, in order for antimony pentoxide, which is blended as a flame retardant aid, to be stably present in the 7㎱/-l resin varnish, it is desirable that 20% by weight or more of the solvent in the varnish be a water solvent.
このようにして紙基材に五酸化アンチモン入りの７エノ
ール系樹脂フエスを一次含浸するが、この−次含浸にお
いて紙基材への五酸化アンチモンの付着量は紙基材に対
して０．２〜１０重且％に設定されるのが好ましい。０
．２重量％未満の場合は難燃効果の発揮が不十分であり
、また１０重量％を超えると積層板製品の機械的強度が
低下する傾向を生じる。また紙基材に対する７エ７−ル
系樹脂の付着量は５〜２０重量％に設定されるのが好ま
しい。５重量％未満の場合は積層板製品の耐湿性や電気
特性の向上が不十分であり、また２０重量％を超えると
二次以降の樹脂含浸（本含浸）が困難になる傾向を生じ
る。In this way, the paper base material is primarily impregnated with the 7-enol resin FES containing antimony pentoxide, but in this second impregnation, the amount of antimony pentoxide attached to the paper base material is 0.2% of the paper base material. It is preferable to set it to 10% by weight. 0
．． If it is less than 2% by weight, the flame retardant effect is insufficient, and if it exceeds 10% by weight, the mechanical strength of the laminate product tends to decrease. Further, it is preferable that the amount of the 7-el resin adhered to the paper base material is set to 5 to 20% by weight. If it is less than 5% by weight, the moisture resistance and electrical properties of the laminate product will not be sufficiently improved, and if it exceeds 20% by weight, secondary resin impregnation (main impregnation) will tend to become difficult.
上記のようにして一次含浸がなされた紙基材にさらに樹
脂ワニスを含浸させる。この二次以降に含浸されるワニ
スの含浸樹脂としては特に限定されるものではないが、
例えばフエ／−ル８（脂、エポキシ樹脂、ポリエステル
樹脂、メラミン樹脂などを挙げることができる。またこ
の二次以降に含浸される樹脂ワニスにはハロゲン化合物
を添加するかあるいはハロゲン化合物で変性した樹脂を
用いる必要がある。このように二次以降の含浸をおこな
ったのちに紙基材を乾燥することによって樹脂含浸基材
を得ることができる。The paper base material that has been primarily impregnated as described above is further impregnated with a resin varnish. The impregnating resin for the varnish that is impregnated after this secondary stage is not particularly limited, but
For example, fer/8 resin, epoxy resin, polyester resin, melamine resin, etc. can be mentioned.In addition, a halogen compound is added to the resin varnish that is impregnated from this secondary stage onwards, or a resin modified with a halogen compound is used. A resin-impregnated base material can be obtained by drying the paper base material after performing the secondary impregnation in this way.
次に本発明を実施例によってさらに説明する。Next, the present invention will be further explained by examples.
叉Ｊｕｌ
フェノールとホルマリンを主成分とするレゾール型７エ
／−ル樹脂１００重量部、水４００重１部、メタノール
５００重量部、固形分４８％の五酸化アンチモンゾル（
８産化学工業製）５０重量部からなる溶液によって樹脂
ワニスを調製し、直ちにこれを厚み１０ミルスのクラ７
）紙に一次含浸させた。これを１２０℃の乾燥機中で１
５分間乾燥し、五酸化アンチモンとフェノール樹脂とが
付着した紙基材を得た。このときの紙基材中の五酸化ア
ンチモンの付着量は紙基材に対して３重量％、フェノー
ル樹脂の付着量は紙基材に対して１２重量％であった。100 parts by weight of resol type 7 ether resin whose main components are phenol and formalin, 400 parts by weight of water, 500 parts by weight of methanol, antimony pentoxide sol with a solid content of 48% (
A resin varnish was prepared using a solution consisting of 50 parts by weight (manufactured by 8 San Kagaku Kogyo), and this was immediately applied to a 10 mils thick varnish.
) The paper was primarily impregnated. This was dried in a dryer at 120℃ for 1
After drying for 5 minutes, a paper base material to which antimony pentoxide and phenol resin were adhered was obtained. At this time, the amount of antimony pentoxide adhered to the paper base material was 3% by weight, and the amount of phenol resin adhered to the paper base material was 12% by weight.
つぎにフェノールとホルマリンと桐油とを主成分とする
レゾール樹脂にテトラブロムフェノールＡ（以下ＴＢＡ
と略称）をレゾール樹脂に対して２５重量％添加してフ
ェノール樹脂ワニスを調製し、これを−犬舎浸を完了し
た上記紙基材に二次含浸として含浸させて乾燥し、樹脂
含有量が５３重１％の樹脂含浸基材を得た。Next, tetrabromophenol A (hereinafter referred to as TBA) is added to a resol resin whose main components are phenol, formalin, and tung oil.
A phenolic resin varnish is prepared by adding 25% by weight of 25% by weight of 25% by weight of the resol resin, and this is impregnated as a secondary impregnation onto the above-mentioned paper base material which has been soaked in the kennel and dried to reduce the resin content. A resin-impregnated base material having a weight of 53 and 1% was obtained.
叉１１」−
フェノールとホルマリンを主成分とするレゾール型フェ
ノール樹脂１００重量部、水３３０重量部、アセトン４
００重量部、固形分４８％の五酸化アンチモンゾル（８
産化学工業１３０重量部からなる溶液によって樹脂ワニ
スを調製し、直ちに゛これを厚み１０ミルスのリンター
紙に一次含浸させた。これを１２０℃の乾燥機中で１５
分間乾燥し、五酸化アンチモンと７エノール樹脂とが付
着した紙基材を得た。このとトの紙基材中の五酸化アン
チモンの付着量は紙基材に対して２重量％、フェノール
樹脂の付着量は紙基材に対して１５重量％であった。11'' - 100 parts by weight of resol type phenolic resin whose main components are phenol and formalin, 330 parts by weight of water, 4 parts by weight of acetone
00 parts by weight, 48% solids antimony pentoxide sol (8
A resin varnish was prepared using a solution containing 130 parts by weight of Sankagaku Kogyo Co., Ltd., and was immediately impregnated onto linter paper having a thickness of 10 mils. This was dried in a dryer at 120℃ for 15 minutes.
It was dried for a minute to obtain a paper substrate to which antimony pentoxide and 7-enol resin were adhered. The amount of antimony pentoxide adhered to the paper base material in this case was 2% by weight, and the amount of phenol resin adhered to the paper base material was 15% by weight.
つぎにエポキシ樹＊＜大日本インキ化学工業製エピクロ
ン８６０）１００重量部、ブロム化エポキシ樹脂（大日
本インキ化学工業製エビクロン１５３）３０重量部、フ
シフンジアミド５重量部、ベンジルツメチルアミン０．
１重量部を含有するエポキシ樹脂ワニスを調製し、これ
を−犬舎浸を完了した上記紙基材に二次含浸として含浸
させて乾燥し、樹脂含有量が５４重量％の樹脂含浸基材
を得た。Next, 100 parts by weight of epoxy tree *<Epiclon 860 manufactured by Dainippon Ink Chemical Industries, Ltd.), 30 parts by weight of brominated epoxy resin (Epiclon 153 manufactured by Dainippon Ink Chemical Industries), 5 parts by weight of fusifundiamide, and 0.0 parts by weight of benzyltumethylamine.
An epoxy resin varnish containing 1 part by weight was prepared, and this was impregnated as a secondary impregnation into the above-mentioned paper substrate which had undergone kennel soaking, and dried to form a resin-impregnated substrate having a resin content of 54% by weight. Obtained.
犬１１」一
実施例１における五酸化７ンチモンと７エノール樹脂を
配合した樹脂ワニスを２４時間放置したのちに、この樹
脂ワニスを紙基材に一次含浸として含浸させるようにし
た他は実施例と同様にして樹脂含浸基材を得た。このと
き−大会没後の紙基材中での五酸化アンチモンの付着量
は紙基材に対して３重量％、フェノール樹脂の付着量は
紙基材に対して１２重１％で、実施例１と同じであった
。Dog 11'' 1 Example 1 except that the resin varnish containing 7 timony pentoxide and 7 enol resin in Example 1 was allowed to stand for 24 hours, and then the paper base material was impregnated with this resin varnish as the primary impregnation. A resin-impregnated base material was obtained in the same manner. At this time, the amount of antimony pentoxide adhered to the paper base material after the event was 3% by weight based on the paper base material, and the amount of phenol resin adhered to the paper base material was 12% by weight. It was the same.
このことは五酸化アンチモンとフェノール樹脂を含有す
る樹脂ワニスは安定した状態を保つことを意味する。This means that the resin varnish containing antimony pentoxide and phenolic resin remains stable.
一次含浸用の樹脂ワニスに五酸化７ンチモンを１００重
量部配合するようにした他は実施例１と同様にして樹脂
含浸基材を得た。このとき−大会没後の紙基材中の五酸
化アンチモンの付着量は紙基材に対して６重量％であっ
た。A resin-impregnated base material was obtained in the same manner as in Example 1, except that 100 parts by weight of 7thimony pentoxide was added to the resin varnish for primary impregnation. At this time, the amount of antimony pentoxide deposited on the paper base material after the competition was 6% by weight based on the paper base material.
夾１１」−
一次含浸用の樹脂ワニスに五酸化７ンチモンを２０重量
部配合するようにした他は実施例１と同様にして樹脂含
浸基材を得た。このとき−犬舎没後の紙基材中の五酸化
アンチモンの付着量は紙基材に対して１重１％であった
。11'' - A resin-impregnated base material was obtained in the same manner as in Example 1, except that 20 parts by weight of 7-thimony pentoxide was added to the resin varnish for primary impregnation. At this time, the amount of antimony pentoxide adhered to the paper base material after the kennel had died was 1% by weight based on the paper base material.
Ｋ１涯１
一次含浸用の樹脂ワニスに五酸化アンチモンの代わりに
三酸化７ンチモンを３０重量部配合するようにした他は
実施例１と同様にして樹脂含浸基材を得た。このとき−
犬舎没後の紙基材中の三酸化アンチモンの付着量は紙基
材に対して３重量％であった。K1 Life 1 A resin-impregnated base material was obtained in the same manner as in Example 1, except that 30 parts by weight of 7tinymonium trioxide was added to the resin varnish for primary impregnation instead of antimony pentoxide. At this time-
The amount of antimony trioxide adhered to the paper base material after the kennel had died was 3% by weight based on the paper base material.
ルμ［
…Ｗ例目二七は入＝静什アン千モンと７７ノール樹脂を
配合した樹脂ワニスを２４時間放置したのちに、この樹
脂ワニスを紙基材に一次含浸として含浸させるようにし
た他は実施例と同様にして！Ｍ脂含浸基材を得た。この
とき−大会没後の紙１材中での二酸化アンチモンの付着
量は紙基材に対して０．１重量％、フェノール樹脂の付
着量は紙基材に対して１２重量％であった。このことは
三酸化７ンチモンが樹脂ワニス中で沈降したことを意味
する。Leμ[...W Example 27 is entered=Shizuki Ann Senmon and 77 After leaving the resin varnish mixed with Nord resin for 24 hours, this resin varnish was impregnated into the paper base material as a primary impregnation. The rest is the same as the example! A base material impregnated with M fat was obtained. At this time, the amount of antimony dioxide adhered to the paper after the tournament was 0.1% by weight based on the paper base material, and the amount of phenol resin adhered to the paper base material was 12% by weight. This means that the 7th monium trioxide was precipitated in the resin varnish.
ル且１」−
一次含浸用の樹脂ワニスに五酸化アンチモンを配合しな
い池は実施例１と同様にして樹脂含浸基材を得た。1 - A resin-impregnated base material was obtained in the same manner as in Example 1, except that antimony pentoxide was not added to the resin varnish for primary impregnation.
ｚ息１」−
ＴＢＡをレゾール樹脂に対して５０重量％配合して二次
含浸用の樹脂ワニスを調製して用いた他は比較例３と同
様にして樹脂含浸基材を得た。A resin-impregnated base material was obtained in the same manner as in Comparative Example 3, except that 50% by weight of TBA was blended with the resol resin to prepare and use a resin varnish for secondary impregnation.
上記各実施例や各比較例で得た樹脂含浸基材を各８枚積
層すると共にその片側に接着剤付きの銅箔（厚み３５μ
）を積層し、これを加熱加圧成形して印刷記線板用の片
面銅張積層板を得た。この積層板の耐熱特性と難燃特性
を測定した。結果を第１表に示す。第１表中、「半田耐
熱性」は２６０°Ｃの半田浴に積層板を浮かせて７クレ
が発生するまでの時間を測定することによって試験をお
こなっｓ １ 舟（重量％）
第１表の結果、五酸化アンチモンを用いた各実施例のも
のでは耐熱特性を低下させることなく難燃特性を向上で
さることが確Ｂされる。また実施例１と実施例３との比
較によって五酸化アンチモンは樹脂ワニス中で安定に存
在することが確認される。Eight resin-impregnated base materials obtained in each of the above Examples and Comparative Examples were laminated, and one side of the resin-impregnated base materials was laminated with copper foil (thickness: 35 μm) with adhesive.
) were laminated and molded under heat and pressure to obtain a single-sided copper-clad laminate for printing marking boards. The heat resistance and flame retardant properties of this laminate were measured. The results are shown in Table 1. In Table 1, "soldering heat resistance" was tested by floating the laminate in a solder bath at 260°C and measuring the time until 7 cracks occurred. As a result, it is confirmed that each of the examples using antimony pentoxide can improve the flame retardant properties without deteriorating the heat resistance properties. Furthermore, a comparison between Example 1 and Example 3 confirms that antimony pentoxide exists stably in the resin varnish.
［発明の効果］
上述のように本発明にあっては、五酸化アンチモンが配
合された７工７−ル系樹脂ワニス全紙基材に一次含浸さ
せたのちに、ハロゲン化合物を含む樹脂ワニスを紙基材
に含浸させ、これを乾燥するようにしたものであるから
、五酸化アンチモンを用いることでハロゲン化合物の使
用量を低減して耐熱特性を低下させることなく難燃特性
を向上させることができるものであり、しがも五酸化ア
ンチモンはフェノール系樹犯ワニス中で均一に沈降され
ることなく分散されるものであり、難燃特性を安定して
向上させることができるものである。[Effects of the Invention] As described above, in the present invention, after the entire paper base material is first impregnated with a 7-l resin varnish containing antimony pentoxide, the resin varnish containing a halogen compound is applied to the paper. Since it is impregnated into a base material and then dried, antimony pentoxide can be used to reduce the amount of halogen compounds used and improve flame retardant properties without reducing heat resistance. However, antimony pentoxide is uniformly dispersed in the phenolic varnish without being precipitated, and can stably improve flame retardant properties.
Claims (2)
ワニスを紙基材に一次含浸させたのちに、ハロゲン化合
物を含む樹脂ワニスを紙基材に含浸させ、これを乾燥す
ることを特徴とする樹脂含浸基材の製造方法。(1) A resin characterized by first impregnating a paper base material with a phenolic resin varnish containing antimony pentoxide, then impregnating the paper base material with a resin varnish containing a halogen compound, and drying this. Method for producing impregnated base material.
ワニスはその溶媒の２０重量％以上が水であることを特
徴とする特許請求の範囲第１項記載の樹脂含浸基材の製
造方法。(2) The method for producing a resin-impregnated base material according to claim 1, wherein the phenolic resin varnish containing antimony pentoxide contains water at least 20% by weight of its solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13898186A JPH072853B2 (en) | 1986-06-14 | 1986-06-14 | Method for producing resin-impregnated base material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13898186A JPH072853B2 (en) | 1986-06-14 | 1986-06-14 | Method for producing resin-impregnated base material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62295929A true JPS62295929A (en) | 1987-12-23 |
| JPH072853B2 JPH072853B2 (en) | 1995-01-18 |
Family
ID=15234688
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13898186A Expired - Lifetime JPH072853B2 (en) | 1986-06-14 | 1986-06-14 | Method for producing resin-impregnated base material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH072853B2 (en) |
-
1986
- 1986-06-14 JP JP13898186A patent/JPH072853B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH072853B2 (en) | 1995-01-18 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |