JPS58179216A - Preparation of phenolic resin - Google Patents
Preparation of phenolic resinInfo
- Publication number
- JPS58179216A JPS58179216A JP6345082A JP6345082A JPS58179216A JP S58179216 A JPS58179216 A JP S58179216A JP 6345082 A JP6345082 A JP 6345082A JP 6345082 A JP6345082 A JP 6345082A JP S58179216 A JPS58179216 A JP S58179216A
- Authority
- JP
- Japan
- Prior art keywords
- formaldehyde
- phenol
- ratio
- phenolic resin
- reaction
- 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.)
- Pending
Links
Landscapes
- Phenolic Resins Or Amino Resins (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は化粧板や積層板等に使用される水溶性のフェノ
ール樹脂の製造法に関するものであるう従来より化粧板
や積層板等に使用されるフェノール樹脂としては、メタ
ノール等の有機溶剤に溶解させたフェノール樹脂が一般
には使用されているが、この本のでは作業時に4を機溶
剤が蒸発するために公害の面より好ましい本のではなく
、またコストも妬くなるという欠点があるため最近では
水を溶媒とした水溶性のフェノール樹脂が使用される傾
向にある。しかし乍ら、水溶性フェノール樹脂を製造す
るKあたって、フェノールとホルムアルデヒドとの反応
がすすんでフェノール樹脂の分子量が増大すると、水に
は溶けなくなるという問題があるため、従来よりフェノ
ールと本ルムアルチしドとの反応に際して種々の検討が
成されている。その手段としては、フェノールに対する
ホルムアルデヒドのtシ比を増して〔約1.5亡シ以上
〕フェノール樹脂の分子量の増大を抑える方法、反応時
間を延長する方法、バラ配合性の強い触媒を用いる方法
、低温(90℃以下)で反応させる方法等があるが、い
ずれ本得られたフェノール樹脂の性能及び収率が緻く満
足のいく本のではなかった。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a water-soluble phenolic resin used for decorative laminates, laminates, etc. Conventionally, phenolic resins used for decorative laminates, laminates, etc. include: Generally, phenolic resins dissolved in organic solvents such as methanol are used, but in this book, the organic solvent evaporates during work, so it is not a preferable book in terms of pollution, and it is also costly. Because of this drawback, there has recently been a tendency to use water-soluble phenolic resins that use water as a solvent. However, when producing water-soluble phenolic resins, there is a problem in that when the reaction between phenol and formaldehyde progresses and the molecular weight of the phenolic resin increases, it becomes insoluble in water. Various studies have been conducted regarding the reaction with The methods include increasing the ratio of formaldehyde to phenol (more than about 1.5%) to suppress the increase in the molecular weight of the phenol resin, extending the reaction time, and using a catalyst with strong dispersion properties. However, the performance and yield of the phenol resin obtained were not satisfactory due to poor performance and yield.
未発明は上記の点Kflliみて成されたものであって
、収率が高くしかも性能に優れた水溶性のフェノールm
脂の製造法を提供することを目的とするものである。The uninvented invention was made in view of the above points, and it is a water-soluble phenol m with high yield and excellent performance.
The purpose of this invention is to provide a method for producing fat.
以ト本発用を詳述する。才ず初めに、フェノールとホル
ムアルデヒドとをホルムアルデヒド/フェノールのtL
比が0.3〜0.6になるように設定して反応さゼる。This publication is detailed below. At the beginning, phenol and formaldehyde are combined into tL of formaldehyde/phenol.
The reaction is carried out by setting the ratio to be 0.3 to 0.6.
このようにすると、フェノールに対するホルムアルデヒ
ドのV:L比が小さいためにホルムアルデヒドとフェノ
ールとの反応は一定の−“合度で止まり、長時間反応さ
せてもゲル化することがないものである。また、そのた
め得られた反応物の分子量分布はシャープになるもので
ある・フェノールに対するホルムアルデヒドのでL比が
0.3未満の場合には反応がほとんど進行しないもので
あり、また、0.6會超える場合には反応物の分子量が
増大して油溶化し、水溶性の樹脂として汀収率が減少す
るものである0次に、このようK して得らhた反応物
にホルムアルデヒドを加えてホルムアルデヒド/フェノ
ールのtL比t−0゜9〜1.3ニなるように設定して
反応させ、フェノ−L樹脂を得る。ここで、フェノール
に対するホルムアルデヒドのEL比が0.9未満の場合
には反応性が慈くて収率が低下するものであり、鵞たl
。In this way, since the V:L ratio of formaldehyde to phenol is small, the reaction between formaldehyde and phenol stops at a certain degree, and gelation does not occur even if the reaction is allowed to occur for a long time. Therefore, the molecular weight distribution of the obtained reactant becomes sharp. -Since formaldehyde is relative to phenol, if the L ratio is less than 0.3, the reaction will hardly proceed, and if it exceeds 0.6, the reaction will hardly proceed. The molecular weight of the reactant increases and it becomes oil-solubilized, resulting in a decrease in slag yield as a water-soluble resin.Next, formaldehyde is added to the reaction product obtained in this manner to form formaldehyde/phenol. The reaction is carried out by setting the tL ratio t-0° of 9 to 1.3d to obtain a pheno-L resin.Here, if the EL ratio of formaldehyde to phenol is less than 0.9, the reactivity is Unfortunately, the yield will decrease, and the
.
3を超える場合に4収率が低下する本のである。This book shows that the yield of 4 decreases when it exceeds 3.
しかして、このようにして得らhたフェノール樹脂はホ
ストフオーム用の樹脂として主に使用さh、化粧板や積
層板等の製造に利用される。フェノール樹脂を水に溶解
したフェノール樹脂ワニスは無公害であり、才だ低コス
トであるのけもちろんのこと、積層板用のクラフト紙等
に対してもメタノール溶解フェノール樹脂ワニスに比し
て浸透性が良し/’1本のである。また、フェノール樹
脂りニス中のフェノール樹脂の分子量分布がシャープで
あるために各特性に優ね、このフェノール樹脂ワニスを
使用して成形された積層板は耐熱性にも優りている本の
である。The phenolic resin thus obtained is mainly used as a resin for host foams, and is used in the production of decorative boards, laminates, and the like. Phenol resin varnish, which is made by dissolving phenolic resin in water, is not only non-polluting and inexpensive, but also has better permeability to kraft paper for laminates than methanol-dissolved phenol resin varnish. It's good/'It's one piece. Additionally, because the molecular weight distribution of the phenolic resin in the phenolic resin varnish is sharp, it has excellent properties, and laminates molded using this phenolic resin varnish also have excellent heat resistance.
上記のように末完明け、フェノールとホルムアルデヒド
とをtL比でホルムアルヂしド/フェノールが0.3〜
0.6になるようVC設定して反応せしめ、次いでこの
反応物にホルムアルデヒドを加えてtL比でホルムアル
デヒド/フェノールが0.9〜1.3になるように設定
して反応せしめたので、@lの段階でフェノールをフェ
ノールに対する0゜3〜0.6tルのホルムアルデヒド
と反応させることによりゲル化することなく低分子量の
水溶性の反応物を高収率で得、次いで4M2段階でこの
反応物にホルムアルチしド/フェノールの℃L比が09
〜1.3になるようにホルムアルデヒドを加えて反応せ
しめることで水に溶ける程度に重合されたフェノール樹
脂を高収率で得ることができ、水溶性フェノール樹脂の
生産性を向上することができる本のである◎
以F未発明を実施例により具体的に説明する。As mentioned above, the formaldehyde/phenol ratio in tL is 0.3~
The reaction was carried out by setting the VC to 0.6, and then formaldehyde was added to this reaction product, and the reaction was carried out by setting the formaldehyde/phenol ratio to be 0.9 to 1.3 in tL, so @l A low molecular weight, water-soluble reactant was obtained in high yield without gelation by reacting phenol with 0.3 to 0.6 t of formaldehyde relative to the phenol in the step, and then this reactant was reacted in a 4M2 step. Formaltide/phenol ℃L ratio is 09
This book can improve the productivity of water-soluble phenolic resins by adding formaldehyde to a reaction temperature of ~1.3 to obtain a polymerized phenolic resin that is soluble in water in high yield. ◎ Hereinafter, the invention will be specifically explained with reference to Examples.
〈実施例1〉
ホルムアルヂしド々してパラホルムを水で561鎗%濃
度に希釈したものを使用し、ホルムアルデヒド/フェノ
ールのtL比を0.5に設定して水酸化ナトリウムでp
Hを9.0Kil整し1、還流温度で100分間反応さ
せた。次に、この反応物に37%ホルマリシ溶液を加え
てホルムアルデヒド/フェノールのtL比を1.OK!
Il整し、還流温度で30分間反応させてフェノール樹
脂ワニスを得た。フェノール樹脂の収率r176%であ
った。<Example 1> Using formaldehyde, paraform was diluted with water to a concentration of 561%, and the formaldehyde/phenol tL ratio was set to 0.5, and the mixture was diluted with sodium hydroxide.
9.0Kil of H was prepared and reacted at reflux temperature for 100 minutes. Next, 37% formalisin solution was added to the reaction to bring the formaldehyde/phenol tL ratio to 1. OK!
After adjusting the temperature, the mixture was reacted at reflux temperature for 30 minutes to obtain a phenol resin varnish. The yield of phenol resin was 176%.
く比較例1〉
ホルムアルゲしド/フェノールのtL比を1. OK&
定すると共に水酸化ナトリウムでpHを9.0Kfjg
整し、還流温度で40分間反応させてフェノール樹脂ワ
ニスを得た。フェノール樹脂の収率け6296であった
。Comparative Example 1> Formalgide/phenol tL ratio was 1. OK&
and adjust the pH to 9.0 Kfjg with sodium hydroxide.
The mixture was then reacted at reflux temperature for 40 minutes to obtain a phenol resin varnish. The yield of phenolic resin was 6296.
く比較例2〉
比較例1で得た樹脂をさら[85℃で180分間反応さ
せてフェノール樹脂ワニスを得た。フェノール樹脂の収
率tf6g%であった。Comparative Example 2> The resin obtained in Comparative Example 1 was further reacted at 85° C. for 180 minutes to obtain a phenolic resin varnish. The yield of phenol resin was tf 6g%.
〈実施例2〉
樹脂量50重壷¥のメラニン樹脂ワニスを薄葉紙に含浸
・乾燥して得たオーバレイづリプレジ1枚と、同上のメ
ラニン樹脂ワニスをパターン紙に含浸−乾燥して得たパ
ターン紙つりづレジ1枚と1で得た樹脂量50m置ぢの
水溶性フェノール樹脂ワニスをクラフト紙に含浸・乾燥
して得たコア一つりづレジ4枚を積層し、この積層体を
金型づレートに挾んで160℃、100Kt/−の条件
にて60分間圧縮成形してメラミン化粧板を得た。<Example 2> One overlay sheet obtained by impregnating thin paper with melanin resin varnish with a resin amount of 50 yen and drying it, and a pattern paper obtained by impregnating pattern paper with the same melanin resin varnish and drying it. Laminate one Tsurizuregi and four core Tsurizuregi obtained by impregnating kraft paper with the water-soluble phenolic resin varnish obtained in step 1 and drying the resin amount of 50 m, and mold this laminate. A melamine decorative board was obtained by compression molding for 60 minutes at 160° C. and 100 Kt/−.
く比較例3〉
比較例1で得たフェノール樹脂ワニスをクラフト紙に含
浸・乾燥して得たファープリプレクを使用した他は実施
例2と同様にしてメラミン化粧板を得た。Comparative Example 3 A melamine decorative board was obtained in the same manner as in Example 2, except that fur prepurek obtained by impregnating and drying kraft paper with the phenolic resin varnish obtained in Comparative Example 1 was used.
〈比較例4〉
比較例2で得たフェノール樹脂ワニスをクラフト紙に含
浸・乾燥して得たコアーづリプレフを使用した他は実施
例2と同様にしてメラミン化粧板を得た。<Comparative Example 4> A melamine decorative board was obtained in the same manner as in Example 2, except that a cored lipure obtained by impregnating and drying kraft paper with the phenolic resin varnish obtained in Comparative Example 2 was used.
次に、実施例2及び比較例3.4で得た化粧板上[18
0℃の油を入れた金属製容器を20分間放置し、その後
の熱劣化を測定した。その結果、いずれの化粧板も異常
は見られなかった。このことから、実施例1で得たフェ
ノール樹脂ワニスにあっては、高収率で製造できるVc
4かかわらず、耐熱性は従来と同等の性能を有している
ことがわかる。Next, on the decorative board obtained in Example 2 and Comparative Example 3.4 [18
A metal container containing oil at 0° C. was left for 20 minutes, and thermal deterioration thereafter was measured. As a result, no abnormality was found in any of the decorative boards. From this, it can be seen that the phenolic resin varnish obtained in Example 1 has Vc
4, it can be seen that the heat resistance performance is equivalent to that of the conventional method.
Claims (1)
ホルムアルデヒド/フェノールが0.3〜0.6 Kな
るように設定して反応せしめ、次いでこの反応物にホル
ムアルデヒドを加えて七シ比でホルムアルデヒド/フェ
ノールが0.9〜1.3になるように設定して反応せし
めることを特徴とするフェノール樹脂の製造法。111 Phenol and formaldehyde are reacted at a temperature ratio of 0.3 to 0.6 K, and then formaldehyde is added to the reaction mixture to react with formaldehyde/phenol at a ratio of 7 °C. A method for producing a phenol resin, characterized in that the reaction is carried out by setting the ratio to 0.9 to 1.3.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6345082A JPS58179216A (en) | 1982-04-15 | 1982-04-15 | Preparation of phenolic resin |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6345082A JPS58179216A (en) | 1982-04-15 | 1982-04-15 | Preparation of phenolic resin |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS58179216A true JPS58179216A (en) | 1983-10-20 |
Family
ID=13229585
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP6345082A Pending JPS58179216A (en) | 1982-04-15 | 1982-04-15 | Preparation of phenolic resin |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS58179216A (en) |
-
1982
- 1982-04-15 JP JP6345082A patent/JPS58179216A/en active Pending
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