JPH08157634A - Production of expanded water-absorbing phenolic resin article - Google Patents
Production of expanded water-absorbing phenolic resin articleInfo
- Publication number
- JPH08157634A JPH08157634A JP34115094A JP34115094A JPH08157634A JP H08157634 A JPH08157634 A JP H08157634A JP 34115094 A JP34115094 A JP 34115094A JP 34115094 A JP34115094 A JP 34115094A JP H08157634 A JPH08157634 A JP H08157634A
- Authority
- JP
- Japan
- Prior art keywords
- phenolic resin
- foaming agent
- water
- phenol resin
- absorbing
- 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.)
- Withdrawn
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】生花用剣山及び植物の育床等の用
途に使用される吸水性のあるフェノール樹脂発泡体に関
する。TECHNICAL FIELD The present invention relates to a water-absorbent phenolic resin foam used for applications such as Kenzan for fresh flowers and growing beds of plants.
【０００２】[0002]
【従来の技術】一般に液状フェノール樹脂より吸水性フ
ェノール樹脂発泡体を得る場合、フェノール樹脂として
はレゾール型フェノール樹脂が用いられる。発泡剤とし
てはトリクロロトリフルオロエタン（ＣＦＣ−１１
３）、トリクロロモノフルオロメタン（ＣＦＣ−１
１）、ジクロロトリフルオロエタン（ＨＣＦＣ−１２
３）、ジクロロフルオロエタン（ＨＣＦＣ−１４１
ｂ）、等のハロゲン化炭化水素やその誘導体が一般に用
いられる。添加剤としては整泡剤としての界面活性剤、
顔料等が用いられる。硬化剤としては有機酸又はその溶
液及び無機酸が用いられる。これらの原料を均一に混合
しモールド等に散布又は注入し発泡硬化させ吸水性フェ
ノール樹脂発泡体を得る方法が一般的に知られている。
発泡剤として、上記ハロゲン化炭化水素やその誘導体を
用いる場合、これらの発泡剤は引火点がなく製造工程が
安全である。しかしＣＦＣ−１１３，ＣＦＣ−１１等は
極めて安定な化合物であるため対流圏で分解されること
なく成層圏まで到達し、成層圏で紫外線により分解して
塩素原子を放出し、この塩素原子が成層圏のオゾンを分
解しオゾン層の破壊を引き起こすという地球レベルでの
環境破壊の原因として現在世界的に問題になっており
「モントリオール議定書」で特定フロンとして規定され
ており、既に製造及び使用量の規制が世界的に進められ
ている。このためＣＦＣ−１１３，ＣＦＣ−１１等の使
用は規制に従って削減し、他の発泡剤等に代替し全廃し
ていく必要がある。又、ＨＣＦＣ−１２３，ＨＣＦＣ−
１４１ｂ等も分子中に塩素原子を含むため、ＣＦＣ−１
１３，ＣＦＣ−１１に比べて小さいがオゾンを分解する
能力を有しているため、将来的には削減、全廃の方向に
ある。2. Description of the Related Art Generally, when a water-absorbent phenol resin foam is obtained from a liquid phenol resin, a resol type phenol resin is used as the phenol resin. Trichlorotrifluoroethane (CFC-11) is used as a foaming agent.
3), trichloromonofluoromethane (CFC-1)
1), dichlorotrifluoroethane (HCFC-12
3), dichlorofluoroethane (HCFC-141
Halogenated hydrocarbons such as b) and their derivatives are generally used. As an additive, a surfactant as a foam stabilizer,
A pigment or the like is used. As the curing agent, an organic acid or a solution thereof and an inorganic acid are used. A method is generally known in which these raw materials are uniformly mixed, sprayed or poured into a mold or the like, and foam-cured to obtain a water-absorbing phenol resin foam.
When the above-mentioned halogenated hydrocarbon or its derivative is used as the foaming agent, these foaming agents have no flash point and the manufacturing process is safe. However, since CFC-113, CFC-11, etc. are extremely stable compounds, they reach the stratosphere without being decomposed in the troposphere and are decomposed by ultraviolet rays in the stratosphere to release chlorine atoms, and the chlorine atoms release ozone in the stratosphere. As a cause of global environmental damage such as decomposition and destruction of the ozone layer, it is currently a global problem and is specified as a specified CFC in the “Montreal Protocol”. Is being advanced to. For this reason, it is necessary to reduce the use of CFC-113, CFC-11, etc. in accordance with regulations and replace them with other foaming agents, etc. and eliminate them altogether. Also, HCFC-123, HCFC-
Since 141b and the like also contain a chlorine atom in the molecule, CFC-1
13, which is smaller than CFC-11 but has the ability to decompose ozone, so it is in the direction of reduction and total elimination in the future.
【０００３】[0003]
【発明が解決しようとする課題】オゾン破壊係数（ＯＤ
Ｐ：Ｏｚｏｎｅ Ｄｅｐｌｅｔｉｎｇ Ｐｏｔｅｎｔｉ
ａｌ）の大きいハロゲン化炭化水素を使用せずに、地球
レベルでの環境破壊という問題を大幅に改善しつつかつ
その発泡剤に適合した液状フェノール樹脂を用いること
で、成型性及び品質を大幅に改善した吸水性フェノール
樹脂発泡体を製造する方法を提供することにある。Problems to be Solved by the Invention Ozone depletion potential (OD
P: Ozone Depleting Potenti
By using a liquid phenolic resin that is compatible with the foaming agent, it is possible to significantly improve the moldability and quality while using a halogenated hydrocarbon with a large It is an object of the present invention to provide a method for producing an improved water absorbent phenolic resin foam.
【０００４】[0004]
【課題を解決するための手段】上記課題を解決するため
に鋭意研究した結果本発明に到達したもので、すなわち
本発明は液状フェノール樹脂、発泡剤、添加剤及び硬化
剤より吸水性フェノール樹脂発泡体を製造する方法にお
いて、発泡剤としてノルマルペンタン及びイソヘキサン
の混合物を使用し、ノルマルペンタン及びイソヘキサン
の混合比率が７０／３０〜３０／７０であり、液状フェ
ノール樹脂の重量平均分子量が６００〜１０００で水分
含有量が７〜１１％であるフェノール樹脂発泡体の製造
方法である。Means for Solving the Problems The present invention has been achieved as a result of intensive research for solving the above problems, that is, the present invention is a foaming of a water-absorbing phenolic resin from a liquid phenol resin, a foaming agent, an additive and a curing agent. In the method for producing a body, a mixture of normal pentane and isohexane is used as a blowing agent, the mixing ratio of normal pentane and isohexane is 70/30 to 30/70, and the weight average molecular weight of the liquid phenol resin is 600 to 1000. A method for producing a phenol resin foam having a water content of 7 to 11%.
【０００５】本発明を具体的に説明する。本発明に使用
する発泡剤はノルマルペンタンとイソヘキサンである
が、ノルマルペンタンは沸点は３６．１℃で発泡剤とし
ては好適であるが、引火点は−４３℃で引火性であるた
め単独で使用しにくい。しかも単独で使用するとセルが
大きくなる。ノルマルペンタンと混合して使用する炭化
水素を種々検討した結果、イソヘキサンが効果があるこ
とが分かり、本発明に到達したしたわけである。イソヘ
キサン単独で発泡剤として使用すると、沸点が大きいた
め発泡圧が大きくなり成形性が悪くなる。ノルマルペン
タンとイソヘキサンの混合比率は７０／３０〜３０／７
０が望ましく、７０／３０以上の場合は発泡体としての
吸水時間が遅いものになる。３０／７０以下では混合発
泡剤の沸点が高くなり、大きな蒸発潜熱を奪い、発泡圧
が大きくなり、脱型時間が長くなる。発泡剤の総使用量
は特に限定されるものではないが、液状フェノール樹脂
重量部に対して１〜６０重量部、好ましくは４〜４０重
量部とするのがよい。発泡剤が１重量部以下ではフェノ
ール樹脂発泡体としての価値は少なく、発泡剤が６０重
量部を越えるとフェノール樹脂発泡体の細胞が脆弱化し
て使用に耐えられなくなる。尚、本発明の混合発泡剤は
必要に応じて安定剤を添加することも可能である。The present invention will be specifically described. The blowing agents used in the present invention are normal pentane and isohexane. Normal pentane has a boiling point of 36.1 ° C. and is suitable as a blowing agent, but it has a flash point of −43 ° C. and is flammable. Hard to do. Moreover, when used alone, the cell becomes large. As a result of various studies on hydrocarbons used by mixing with normal pentane, it was found that isohexane was effective, and the present invention was achieved. If isohexane is used alone as a foaming agent, the boiling point is large and the foaming pressure becomes large, resulting in poor moldability. The mixing ratio of normal pentane and isohexane is 70/30 to 30/7.
0 is desirable, and when it is 70/30 or more, the water absorption time as a foam becomes slow. When it is 30/70 or less, the boiling point of the mixed foaming agent becomes high, the large latent heat of vaporization is taken, the foaming pressure becomes large, and the demolding time becomes long. The total amount of the foaming agent used is not particularly limited, but it is preferably 1 to 60 parts by weight, and more preferably 4 to 40 parts by weight with respect to the parts by weight of the liquid phenol resin. When the amount of the foaming agent is 1 part by weight or less, the value of the phenol resin foam is small, and when the amount of the foaming agent exceeds 60 parts by weight, the cells of the phenol resin foam become brittle and cannot be used. Incidentally, the mixed foaming agent of the present invention may contain a stabilizer if necessary.
【０００６】本発明に用いる液状フェノール樹脂はフェ
ノール類とアルデヒド類をアルカリ性触媒の存在下で反
応させることによって得られるレゾール型フェノール樹
脂が挙げられるが、本発明に使用する液状フェノール樹
脂としては、重量平均分子量が６００〜１０００でかつ
水分含有量が７〜１１％のものが目標の品質に合致する
ことが分かった。液状フェノール樹脂の重量平均分子量
が６００以下の場合、成形時に発熱反応が急激に進行し
発泡体内部にスコーチ（焼け現象）が発生し、サクサク
として強度が低くなる。又重量平均分子量が１０００以
上の場合、樹脂粘度が高く、攪拌不良となり、たとえ攪
拌を工夫しても反応速度が遅くなり成形性が悪くなる。
加えて液状フェノール樹脂を検討している時に水分含有
量が樹脂化反応に多大な影響があることが分かった。発
泡剤として従来のフロンを使用する場合の液状フェノー
ル樹脂の水分含有量は１２〜１６％と多かった。本発明
の発泡剤を使用する場合は水分含有量は７〜１１％が望
ましいことが分かった。すなわち水分含有量が１１％を
越えた場合は、発泡時の発熱反応による水分の蒸発量が
多いので、その蒸発潜熱による吸熱作用で成形性が悪く
なる。又吸熱作用が低下してから発泡が進んでいくの
で、発泡圧が上昇するまでの時間が長くなる。水分含有
量が７％未満では蒸発潜熱が少ないため、発泡体内部の
温度が上昇しすぎてスコーチ（焼け現象）が発生する。The liquid phenol resin used in the present invention includes a resol type phenol resin obtained by reacting phenols and aldehydes in the presence of an alkaline catalyst. The liquid phenol resin used in the present invention is It was found that those having an average molecular weight of 600 to 1000 and a water content of 7 to 11% meet the target quality. When the weight average molecular weight of the liquid phenol resin is 600 or less, an exothermic reaction rapidly progresses during molding, scorch (burn phenomenon) occurs inside the foam, and the strength becomes crispy and low. On the other hand, when the weight average molecular weight is 1000 or more, the resin viscosity is high, resulting in poor stirring, and even if the stirring is devised, the reaction rate becomes slow and the moldability deteriorates.
In addition, when examining liquid phenolic resins, it was found that the water content had a great influence on the resinification reaction. When conventional freon was used as a foaming agent, the water content of the liquid phenol resin was as high as 12 to 16%. It has been found that a water content of 7 to 11% is desirable when the foaming agent of the present invention is used. That is, when the water content exceeds 11%, a large amount of water evaporates due to an exothermic reaction during foaming, and the endothermic action of the latent heat of evaporation deteriorates moldability. Further, since the endothermic action decreases and the foaming proceeds, the time until the foaming pressure rises becomes long. When the water content is less than 7%, the latent heat of vaporization is small, so the temperature inside the foam rises too much and scorch (burn phenomenon) occurs.
【０００７】添加剤としては公知の界面活性剤、たとえ
ば、シロキサン・オキシアルキレン共重合体、ポリオキ
シエチレンソルビタン脂肪酸エステル、ヒマシ油エチレ
ンオキシド付加物等のノニオン系界面活性剤及びアルキ
ルスルホン酸塩、アルキルベンゼンスルホン酸塩等のア
ニオン系界面活性剤を併用して用いる。硬化剤としては
リン酸、亜リン酸、次亜リン酸、ピロリン酸、トリポリ
リン酸、塩酸、硫酸等の無機酸、フェノールスルホン
酸、トルエンスルホン酸、キシレンスルホン酸、ベンゼ
ンスルホン酸等のアリールスルホン酸やメタンスルホン
酸等のアルキルスルホン酸等の有機酸が用いられるがこ
れに限定されるものではない。又これらの硬化剤は単独
で又は２種以上を併用することも可能であり、水溶液と
して使用することも他の溶液として使用することも或い
は非溶液として使用することも可能である。この硬化剤
の使用量は特に限定されるものではないが、液状フェノ
ール樹脂１００重量部に対して１〜６０重量部、好まし
くは５〜３０重量部とするのがよい。As the additives, known surfactants such as siloxane / oxyalkylene copolymers, polyoxyethylene sorbitan fatty acid esters, castor oil ethylene oxide adducts and other nonionic surfactants, and alkyl sulfonates and alkylbenzene sulfones are used. An anionic surfactant such as an acid salt is used in combination. Examples of the curing agent include inorganic acids such as phosphoric acid, phosphorous acid, hypophosphorous acid, pyrophosphoric acid, tripolyphosphoric acid, hydrochloric acid and sulfuric acid, and arylsulfonic acids such as phenolsulfonic acid, toluenesulfonic acid, xylenesulfonic acid and benzenesulfonic acid. Organic acids such as alkyl sulfonic acid such as and methane sulfonic acid are used, but not limited thereto. Further, these curing agents can be used alone or in combination of two or more kinds, and can be used as an aqueous solution, as another solution, or as a non-solution. The amount of the curing agent used is not particularly limited, but it is preferably 1 to 60 parts by weight, and more preferably 5 to 30 parts by weight with respect to 100 parts by weight of the liquid phenol resin.
【０００８】本発明では、以上に述べた原料を均一に混
合し、引き続きモールド等に散布又は注入し発泡硬化さ
せることによりフェノール樹脂発泡体が得られる。発泡
硬化工程は常温でも加熱雰囲気下でも行うことが可能で
ある。これらの原料の混合はバッチ混合する場合はディ
スパー等の撹拌機が用いられ、連続的に混合する場合は
公知の多成分混合発泡機等が用いられる。In the present invention, the phenol resin foam is obtained by uniformly mixing the above-mentioned raw materials, and then spraying or pouring the mixture into a mold or the like and foam-curing. The foaming and hardening step can be performed at room temperature or under a heated atmosphere. For mixing these raw materials, a stirrer such as a disper is used for batch mixing, and a known multi-component mixing and foaming machine is used for continuous mixing.
【０００９】以下に実施例及び比較例を挙げて本発明に
ついて詳しく説明する。単に部とあるのは重量部を示
す。The present invention will be described in detail below with reference to Examples and Comparative Examples. "Parts" means "parts by weight".
【実施例】フェノール１００部、ホルムアルデヒド３７
％水溶液１７３部及び水酸化リチウム０．５部を反応容
器に投入し、９０℃で所望の重量平均分子量になるまで
反応させ、減圧下に脱水し所望の水分含有量の液状フェ
ノール樹脂を得た。この液状フェノール樹脂１００部に
整泡剤としてシリコン系界面活性剤Ｌ−５４２１（日本
ユニカー製）２部、アニオン系界面活性剤ハイテノール
ＮＥ−０５（第一工業製薬製）２部、発泡剤としてノル
マルペンタン及びイソヘキサンの混合物を発泡体密度が
２１〜２３（kg／m3）になる量を加え均一に攪拌した
後、６５％フェノールスルホン酸水溶液１０部を加えラ
ボミキサーで均一に撹拌混合した後、４０℃の雰囲気温
度に保たれた１００×１００×１００cmの木製モールド
中に流し込み加熱し、３０分後に脱型した。（脱型出来
ないものは１０分間隔で脱型性を確認した）このフェノ
ール樹脂発泡体について目視によりセル状態を観察し、
ＡＳＴＭ Ｄ１６２２に定められた方法で密度と、ＡＳ
ＴＭ Ｄ１６２１に定められた方法で圧縮強度を測定し
た。結果を第１表に示す。[Example] Phenol 100 parts, formaldehyde 37
% Aqueous solution 173 parts and lithium hydroxide 0.5 part were charged into a reaction vessel, reacted at 90 ° C. until a desired weight average molecular weight was obtained, and dehydrated under reduced pressure to obtain a liquid phenol resin having a desired water content. . To 100 parts of this liquid phenol resin, 2 parts of silicone-based surfactant L-5421 (manufactured by Nippon Unicar) as a foam stabilizer, 2 parts of anionic surfactant Hitenol NE-05 (manufactured by Dai-ichi Kogyo Seiyaku Co., Ltd.), and as a foaming agent After adding a mixture of normal pentane and isohexane to a foam density of 21 to 23 (kg / m 3 ) and stirring uniformly, 10 parts of a 65% phenolsulfonic acid aqueous solution was added, and the mixture was uniformly stirred and mixed with a lab mixer. Then, the mixture was poured into a wooden mold of 100 × 100 × 100 cm kept at an ambient temperature of 40 ° C., heated, and demolded after 30 minutes. (For those that could not be demolded, the demolding property was confirmed at intervals of 10 minutes.) The cell state of this phenol resin foam was visually observed,
Density and AS according to the method specified in ASTM D1622
The compressive strength was measured by the method specified in TM D1621. The results are shown in Table 1.
【００１０】[0010]
【表１】 [Table 1]
【００１１】実施例２〜７及び比較例１〜６は第１表に
示すように、発泡剤の種類と割合及び液状フェノール樹
脂の重量平均分子量、水分含有量を変え、その他は実施
例１と同様の方法でフェノール樹脂発泡体を得、同様に
品質の測定を行った。結果を第１表に示す。As shown in Table 1, in Examples 2 to 7 and Comparative Examples 1 to 6, the type and proportion of the foaming agent, the weight average molecular weight of the liquid phenol resin and the water content were changed, and the others were the same as those of Example 1. A phenol resin foam was obtained by the same method, and the quality was measured in the same manner. The results are shown in Table 1.
【００１２】[0012]
【作用】液状フェノール樹脂に、発泡剤としてノルマル
ペンタン／イソヘキサンを７０／３０〜３０／７０の割
合で使用することにより、適正な脱型時間でもって、し
かも均一且つ微細な気泡、早い吸水時間、高い圧縮強度
を有するフェノール樹脂発泡体が得られる。By using normal pentane / isohexane as a foaming agent in the liquid phenol resin at a ratio of 70/30 to 30/70, it is possible to obtain a proper demolding time, uniform and fine bubbles, fast water absorption time, A phenol resin foam having high compressive strength is obtained.
【００１３】[0013]
【発明の効果】本発明で使用されるノルマルペンタン／
イソヘキサンは分子中に塩素原子を含まないためオゾン
を分解しないので安全である。又液状フェノール樹脂が
ノルマルペンタン／イソヘキサンとの相溶性及び沸点等
がフェノール樹脂発泡体の発泡硬化過程での発熱速度、
ゲル化速度等の発泡硬化特性に適合しているため、均一
かつ微細な気泡と優れた物理特性を持つ発泡体が得られ
た。INDUSTRIAL APPLICABILITY Normal pentane used in the present invention /
Isohexane is safe because it does not decompose ozone because it does not contain chlorine atoms in the molecule. Also, the liquid phenolic resin's compatibility with normal pentane / isohexane, the boiling point, etc. are the heat generation rate in the foaming and hardening process of the phenolic resin foam,
Since it is suitable for foaming and hardening characteristics such as gelation rate, a foam having uniform and fine cells and excellent physical properties was obtained.
Claims (2)
剤及び硬化剤より吸水性フェノール樹脂発泡体を製造す
る方法において、発泡剤としてノルマルペンタン及びイ
ソヘキサンの混合物を使用し、該混合物の混合比率（重
量）が７０／３０〜３０／７０であることを特徴とする
吸水性フェノール樹脂発泡体の製造方法。1. A method for producing a water-absorbing phenolic resin foam from a liquid phenolic resin, a surfactant, a foaming agent and a curing agent, wherein a mixture of normal pentane and isohexane is used as a foaming agent, and a mixing ratio of the mixture ( (Weight) is 70/30 to 30/70, the method for producing a water-absorbing phenolic resin foam.
量平均分子量が６００〜１０００で水分含有量が７〜１
１％であることを特徴とする吸水性フェノール樹脂発泡
体の製造方法。2. The liquid phenol resin according to claim 1 has a weight average molecular weight of 600 to 1000 and a water content of 7-1.
It is 1%, The manufacturing method of a water-absorbing phenol resin foam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34115094A JPH08157634A (en) | 1994-12-02 | 1994-12-02 | Production of expanded water-absorbing phenolic resin article |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34115094A JPH08157634A (en) | 1994-12-02 | 1994-12-02 | Production of expanded water-absorbing phenolic resin article |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08157634A true JPH08157634A (en) | 1996-06-18 |
Family
ID=18343723
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34115094A Withdrawn JPH08157634A (en) | 1994-12-02 | 1994-12-02 | Production of expanded water-absorbing phenolic resin article |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08157634A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002046285A1 (en) * | 2000-12-08 | 2002-06-13 | Pool Abdul Kader | Electromagnetic energy adaptation material |
-
1994
- 1994-12-02 JP JP34115094A patent/JPH08157634A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002046285A1 (en) * | 2000-12-08 | 2002-06-13 | Pool Abdul Kader | Electromagnetic energy adaptation material |
| US7344661B2 (en) * | 2000-12-08 | 2008-03-18 | Scott Allan Kuehl | Electromagnetic energy adaptation material |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 20020205 |