JPH1180408A - Preparation of resin foam - Google Patents
Preparation of resin foamInfo
- Publication number
- JPH1180408A JPH1180408A JP9267693A JP26769397A JPH1180408A JP H1180408 A JPH1180408 A JP H1180408A JP 9267693 A JP9267693 A JP 9267693A JP 26769397 A JP26769397 A JP 26769397A JP H1180408 A JPH1180408 A JP H1180408A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- inert gas
- foam
- resin body
- impregnation
- 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
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/3442—Mixing, kneading or conveying the foamable material
- B29C44/3446—Feeding the blowing agent
- B29C44/3453—Feeding the blowing agent to solid plastic material
Landscapes
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、樹脂体に不活性
ガスを含浸させ、ついでこれを加熱して樹脂発泡体を製
造する方法に関し、樹脂体の厚み方向に不活性ガスの含
浸量の濃度勾配を形成することにより、２種の異なるセ
ル構造を同時に有する特殊発泡構造の樹脂発泡体を得る
ようにしたものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a resin foam by impregnating a resin body with an inert gas and then heating the resin body. By forming a gradient, a resin foam having a special foam structure having two different cell structures at the same time is obtained.
【０００２】[0002]
【従来の技術】炭酸ガス等の不活性ガスを熱可塑性樹脂
からなるシート、フィルムなどに液状または超臨界状で
含浸させ、ついでこれを加熱して表面のスキン層と内部
のセル層とからなる樹脂発泡シートなどを得る方法が知
られている。このものは、樹脂シートなどの内部の不活
性ガスの含浸量がその厚み方向にほぼ均一とされるた
め、内部の発泡したセル層のセル構造は、ほぼ均一であ
り、表面のスキン層に近いセル層の部分において若干セ
ル径が小さくなる程度である。2. Description of the Related Art An inert gas such as carbon dioxide is impregnated in a liquid or supercritical state into a sheet or film made of a thermoplastic resin and then heated to form a skin layer on the surface and an internal cell layer. A method for obtaining a resin foam sheet or the like is known. In this case, since the impregnation amount of the inert gas inside the resin sheet or the like is made substantially uniform in the thickness direction, the cell structure of the foamed cell layer inside is almost uniform and close to the skin layer on the surface. The cell diameter is slightly reduced in the cell layer portion.
【０００３】このため、この方法によって製造された樹
脂発泡シートなどでは、機械的特性は均一ではあるもの
の用途が限定され、特殊な用途には不向きであった。ま
た、発泡倍率を高めて樹脂発泡シートなどの低比重化を
図ろうとすると、剛性、曲げ強度などの機械的強度が同
時に低下し、低比重でかつ高機械的強度の樹脂発泡シー
トなどを得ることができなかった。[0003] For this reason, in the resin foam sheet and the like produced by this method, the mechanical properties are uniform, but the use is limited, and it is not suitable for special use. In addition, when attempting to reduce the specific gravity of a resin foam sheet or the like by increasing the expansion ratio, the mechanical strength such as rigidity and bending strength is simultaneously reduced, and a resin foam sheet having a low specific gravity and a high mechanical strength is obtained. Could not.
【０００４】[0004]
【発明が解決しようとする課題】よって、本発明におけ
る課題は、２種の異なるセル構造を有し、これによって
機械的強度の低下を防止しうる特殊発泡構造の樹脂発泡
体を容易に製造できるようにすることにある。SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to easily produce a resin foam having a special foam structure having two kinds of different cell structures and capable of preventing a decrease in mechanical strength. Is to do so.
【０００５】[0005]
【課題を解決するための手段】かかる課題は、樹脂体に
不活性ガスを含浸する際に、樹脂体の厚み方向に不活性
ガスの含浸量の濃度勾配を形成しておき、これを加熱す
る方法によって解決できる。The object of the present invention is to provide a method for impregnating a resin body with an inert gas by forming a concentration gradient of the amount of the inert gas impregnated in the thickness direction of the resin body and heating the same. Can be solved by the method.
【０００６】[0006]
【発明の実施の形態】以下、本発明を詳しく説明する。
本発明で用いられる樹脂体としては、熱可塑性樹脂から
なるフィルム、シート、プレートなどやこれらを成形加
工したものなどが用いられる。熱可塑性樹脂としては、
特に限定されることはなく、ポリエチレン、ポリプロピ
レン、ポリエチレンテレフタレート、ナイロン、ポリテ
トラフルオロエチレン、ポリエーテルエーテルケトン、
ポリアセタールなどの結晶性樹脂、ポリ塩化ビニル、ポ
リスチレン、ポリメチルメタクリレート、ポリカーボネ
ート、ＡＢＳ樹脂、ＡＳ樹脂などの非結晶性樹脂などが
用いられる。また、不活性ガスとしては、樹脂体と化学
反応を起こさない不燃性のガス、例えば炭酸ガス、窒素
ガスなどが用いられ、なかでも液化もしくは超臨界化が
容易な炭酸ガスが好適である。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail.
As the resin body used in the present invention, a film, a sheet, a plate, or the like made of a thermoplastic resin, or a molded product thereof, or the like is used. As a thermoplastic resin,
There is no particular limitation, polyethylene, polypropylene, polyethylene terephthalate, nylon, polytetrafluoroethylene, polyetheretherketone,
A crystalline resin such as polyacetal, a non-crystalline resin such as polyvinyl chloride, polystyrene, polymethyl methacrylate, polycarbonate, ABS resin, and AS resin are used. Further, as the inert gas, a nonflammable gas that does not cause a chemical reaction with the resin body, for example, carbon dioxide gas, nitrogen gas, or the like is used. Among them, carbon dioxide gas that is easily liquefied or supercritical is preferable.
【０００７】具体的な製造方法としては、圧力容器に樹
脂体を入れ、圧力容器内に不活性ガスを導入し、加圧も
しくは加圧、加熱状態として不活性ガスを液状もしくは
超臨界状とし、樹脂体中に含浸させる。樹脂体への不活
性ガスの含浸量は、含浸時の圧力、温度、時間の含浸条
件、樹脂体をなす熱可塑性樹脂の種類、樹脂体の厚みな
どによって変化する。このため、樹脂体の厚み方向での
不活性ガスの含浸量の濃度勾配を形成するには、上記圧
力、温度、時間の含浸条件を適宜定めることによって行
われる。As a specific manufacturing method, a resin body is put into a pressure vessel, an inert gas is introduced into the pressure vessel, and the inert gas is made into a liquid or supercritical state by pressurizing or pressurizing and heating. Impregnated in resin body. The amount of the inert gas impregnated into the resin body varies depending on the impregnation conditions such as the pressure, temperature, and time during the impregnation, the type of the thermoplastic resin forming the resin body, and the thickness of the resin body. Therefore, in order to form a concentration gradient of the amount of impregnation of the inert gas in the thickness direction of the resin body, the impregnation conditions of the above pressure, temperature, and time are appropriately determined.
【０００８】不活性ガスの樹脂体への含浸が、所望の濃
度勾配に達したならば、圧力容器から樹脂体を取り出
し、これを樹脂体をなす樹脂のガラス転移温度以上で溶
融温度以下の温度で、時間１０秒〜５分程度、オイルバ
ス、オーブンなどに入れて加熱し、樹脂体を軟化させる
と同時に内部に含浸されている不活性ガスを気化させて
発泡させる。ついで、この樹脂体を冷水等に浸すなどし
て急速冷却し、気泡の成長を停止させて、目的とする樹
脂発泡体を得る。When the impregnation of the resin body with the inert gas reaches a desired concentration gradient, the resin body is taken out of the pressure vessel and is heated to a temperature not lower than the glass transition temperature of the resin forming the resin body but not higher than the melting temperature. For about 10 seconds to 5 minutes, the resin body is heated in an oil bath or an oven to soften the resin body and vaporize the inert gas impregnated therein to cause foaming. Then, the resin body is rapidly cooled by immersing the resin body in cold water or the like to stop the growth of bubbles to obtain a desired resin foam.
【０００９】図１は、樹脂体の厚み方向の不活性ガス含
浸量の濃度勾配の一例を示すグラフである。この例で
は、樹脂体の厚み方向の中心部分に向けて両表面側から
徐々に含浸濃度が放物線状に低下しているもので、含浸
時の圧力、温度、時間の含浸条件を温和にしたものであ
る。このような濃度勾配を有する樹脂体を加熱して発泡
させた樹脂発泡体は、図２に模式的に示すような特殊な
セル構造を有するものとなる。FIG. 1 is a graph showing an example of the concentration gradient of the amount of inert gas impregnated in the thickness direction of the resin body. In this example, the impregnation concentration gradually decreases in a parabolic manner from both surface sides toward the center in the thickness direction of the resin body, and the impregnation conditions of the impregnation pressure, temperature, and time are mild. It is. A resin foam obtained by heating and foaming a resin body having such a concentration gradient has a special cell structure as schematically shown in FIG.
【００１０】図２において、符号１はスキン層であり、
このスキン層１は樹脂発泡体の両表面層に形成され、実
質的に発泡していない層である。このスキン層１、１の
内側にはそれぞれ微細気泡層２、２が形成されている。
この微細気泡層２は、そのセル径が０．１〜１０μｍ
で、セル密度が１０9〜１０15個／ｃｍ3で、セルの外形
がほぼ球状のものであって、不活性ガス濃度の高い領域
の部分が発泡したものである。また、２つの微細気泡層
２、２に挿まれた中間部分は、細長気泡層３となってい
る。この細長気泡層３は、個々のセルの形状が概略円筒
状となっており、その径（短径）が１０〜１００μｍ、
長さ（長径）が１００〜１０００μｍであり、セル密度
が１０5〜１０9個／ｃｍ3のものであって、不活性ガス
の含浸濃度の低い領域の部分が発泡したものである。In FIG. 2, reference numeral 1 denotes a skin layer,
The skin layers 1 are formed on both surface layers of the resin foam and are not substantially foamed. Fine bubble layers 2 and 2 are formed inside the skin layers 1 and 1, respectively.
This fine bubble layer 2 has a cell diameter of 0.1 to 10 μm.
The cell density is 10 9 to 10 15 cells / cm 3 , the outer shape of the cells is substantially spherical, and the area of the region having a high inert gas concentration is foamed. An intermediate portion inserted between the two fine bubble layers 2 is an elongated bubble layer 3. In the elongated bubble layer 3, the shape of each cell is substantially cylindrical, and the diameter (short diameter) is 10 to 100 μm.
It has a length (major axis) of 100 to 1000 μm, a cell density of 10 5 to 10 9 cells / cm 3 , and foams a part of the region where the concentration of the inert gas impregnated is low.
【００１１】樹脂発泡体の表面に未発泡のスキン層１が
形成される理由は、不活性ガスの含浸後の樹脂体を圧力
容器を取り出した直後から加熱するまでの間に、含浸さ
れている不活性ガスがその表面から速やかに揮散して行
き、その後加熱しても不活性ガスが抜けた表面部分は発
泡しないためである。また、ポリエチレンテレフタレー
トなどの結晶性樹脂を非晶化（アモルファス化）した樹
脂で樹脂体を構成した場合には、不活性ガスの含浸によ
って樹脂のガラス転移温度が低下し、含浸条件下におい
て表面部分から結晶化が進行する。結晶部分は溶融温度
程度にまで加熱しない限り、軟化することはないので、
結晶化した表面部分は発泡せず、スキン層となる。The reason why the unfoamed skin layer 1 is formed on the surface of the resin foam is that the resin body after the impregnation with the inert gas is impregnated immediately after the pressure vessel is taken out and before it is heated. This is because the inert gas volatilizes quickly from the surface, and even if heated thereafter, the surface portion from which the inert gas has escaped does not foam. When the resin body is made of a resin obtained by making a crystalline resin such as polyethylene terephthalate non-crystalline (amorphized), the glass transition temperature of the resin is lowered by impregnation with an inert gas, and the surface portion is impregnated under the impregnation conditions. The crystallization proceeds from. Since the crystal part does not soften unless it is heated to the melting temperature,
The crystallized surface portion does not foam and becomes a skin layer.
【００１２】また、不活性ガス含浸量の大きい部分で
は、この部分を加熱すると、ガスの圧力低下が大きく、
多数の核が発生し、この核に流入するガスの量が少なく
なるため、核から生成するセルは微細で、かつ多数のセ
ルが生成し、これによって微細気泡層２が形成される。
逆に、不活性ガス含浸量の小さい部分では、ガスの圧力
低下が小さく、小数の核が発生し、核に流入するガスの
量が多くなるため、核から生成するセルは大型化し、細
長気泡層３が形成される。In a portion where the amount of inert gas impregnated is large, when this portion is heated, the pressure drop of the gas is large,
Since a large number of nuclei are generated and the amount of gas flowing into the nuclei is reduced, the cells generated from the nuclei are fine and a large number of cells are generated, whereby the fine bubble layer 2 is formed.
Conversely, in the portion where the amount of inert gas impregnated is small, the pressure drop of the gas is small, a small number of nuclei are generated, and the amount of gas flowing into the nuclei increases, so that the cells generated from the nuclei become large and elongated bubbles Layer 3 is formed.
【００１３】図３は、樹脂体の厚み方向の不活性ガス含
浸量の濃度勾配の他の例を示すもので、図１に示したも
のに比べて、含浸条件をさらに温和なものとし、厚み方
向の中央部分には不活性ガスが含浸されていない部分を
形成したものである。図４は、図３に示した濃度勾配を
有する樹脂体を加熱して得られた樹脂発泡体を模式的に
示したもので、このものでは、表面のスキン層１、１の
内側に微細気泡層２、２が形成され、この微細気泡層
２、２の内側には細長気泡層３、３が形成され、これの
内側に未発泡層４が形成されている。未発泡層４は不活
性ガスが含浸されていない部分に対応している。FIG. 3 shows another example of the concentration gradient of the amount of the inert gas impregnated in the thickness direction of the resin body. The impregnation conditions are made milder than those shown in FIG. A portion not impregnated with the inert gas is formed in a central portion in the direction. FIG. 4 schematically shows a resin foam obtained by heating the resin body having the concentration gradient shown in FIG. 3. In this resin foam, fine bubbles are formed inside the skin layers 1 and 1 on the surface. Layers 2 and 2 are formed, and elongated cell layers 3 and 3 are formed inside the fine cell layers 2 and 2, and an unfoamed layer 4 is formed inside these layers. The unfoamed layer 4 corresponds to a portion that is not impregnated with the inert gas.
【００１４】このような樹脂発泡体の製造方法にあって
は、図２および図４に示すような２種の異なるセル構造
を有する特殊発泡構造の樹脂発泡体を、単に不活性ガス
の含浸条件を制御して厚み方向に濃度勾配を形成するだ
けの操作によって、簡単に製造することができる。ま
た、得られる樹脂発泡体は、その特殊な発泡構造に起因
して機械的強度、特に剛性、曲げ強度が高く、しかも低
比重のものとなる。In such a method for producing a resin foam, a resin foam having a special foam structure having two different cell structures as shown in FIGS. 2 and 4 is simply impregnated with an inert gas. Can be easily manufactured by the operation of simply forming a concentration gradient in the thickness direction by controlling the thickness. Further, the obtained resin foam has high mechanical strength, particularly rigidity and bending strength, and low specific gravity due to its special foamed structure.
【００１５】以下、実施例を示して具体的に説明する
が、本発明はこれら実施例に限定されるものではない。Hereinafter, the present invention will be described specifically with reference to examples, but the present invention is not limited to these examples.
【実施例１】樹脂体として、非晶化した厚さ１ｍｍのポ
リエチレンテレフタレートシートを５０×５０ｍｍの大
きさに切断して圧力容器に入れ、密閉した。圧力容器の
温度４０℃に保ちながら、炭酸ガスを導入して圧力容器
内を１２０ａｔｍまで加圧した。圧力容器の温度、圧力
を１５時間保持し、ポリエチレンテレフタレートシート
に炭酸ガスを含浸させた。Example 1 As a resin body, an amorphous polyethylene terephthalate sheet having a thickness of 1 mm was cut into a size of 50 × 50 mm, placed in a pressure vessel, and sealed. While maintaining the temperature of the pressure vessel at 40 ° C., carbon dioxide gas was introduced to pressurize the inside of the pressure vessel to 120 atm. The temperature and pressure of the pressure vessel were maintained for 15 hours, and the polyethylene terephthalate sheet was impregnated with carbon dioxide.
【００１６】１５時間後、圧力容器内の炭酸ガスを放出
して大気圧とし、ポリエチレンテレフタレートシートを
取り出し、このシートを１５０℃のオイルバスに１０秒
間浸して加熱し、発泡させた。以上の操作によって得ら
れた発泡ポリエチレンテレフタレートシートの断面を走
査型電子顕微鏡で観察したところ、図５に示す写真が得
られた。また、発泡シートの全厚みは２．９ｍｍでスキ
ン層の厚みは０．１８ｍｍ、微細気泡層の厚みは０．８
ｍｍ、細長気泡層の厚みは０．９４ｍｍであり、比重は
０．４であった。After 15 hours, carbon dioxide in the pressure vessel was released to atmospheric pressure, the polyethylene terephthalate sheet was taken out, and the sheet was immersed in an oil bath at 150 ° C. for 10 seconds and heated to foam. When the cross section of the foamed polyethylene terephthalate sheet obtained by the above operation was observed with a scanning electron microscope, the photograph shown in FIG. 5 was obtained. The total thickness of the foamed sheet is 2.9 mm, the thickness of the skin layer is 0.18 mm, and the thickness of the fine bubble layer is 0.8.
mm, the thickness of the elongated bubble layer was 0.94 mm, and the specific gravity was 0.4.
【００１７】[0017]
【実施例２】実施例１において、炭酸ガスの含浸時の含
浸時間を１時間とした以外は同様にして発泡ポリエチレ
ンテレフタレートシートを製造した。図６に示す写真
は、この発泡シートの断面構造を示すものである。この
ものでは、含浸時間が短時間であるので、中央部分には
炭酸ガスの未含浸部分に対応する未発泡層が形成されて
いる。また、発泡シートの全厚みは１．５ｍｍで、スキ
ン層の厚みは０．０２５ｍｍ、微細気泡層の厚みは０．
３２ｍｍ、細長気泡層の厚みは０．１８ｍｍ、未発泡層
の厚みは０．４５ｍｍであり、比重は０．５であった。Example 2 A foamed polyethylene terephthalate sheet was produced in the same manner as in Example 1, except that the impregnation time during the impregnation with carbon dioxide gas was changed to 1 hour. The photograph shown in FIG. 6 shows the cross-sectional structure of the foam sheet. In this case, since the impregnation time is short, an unfoamed layer corresponding to the unimpregnated portion of carbon dioxide is formed in the center. The total thickness of the foamed sheet is 1.5 mm, the thickness of the skin layer is 0.025 mm, and the thickness of the fine bubble layer is 0.1 mm.
32 mm, the thickness of the elongated bubble layer was 0.18 mm, the thickness of the unfoamed layer was 0.45 mm, and the specific gravity was 0.5.
【００１８】[0018]
【発明の効果】以上説明したように、本発明の樹脂発泡
体の製法によれば、特殊な発泡構造を有する樹脂発泡体
を極めて簡単な操作によって製造することができる。ま
た、この製法によって得られる樹脂発泡体は、機械的強
度が良好でしかも低比重であり、しかもその特殊な発泡
構造を有することにより、スピーカやマイクロフォンな
どの振動板などの特殊な用途にも使用できる。As described above, according to the method for producing a resin foam of the present invention, a resin foam having a special foam structure can be produced by an extremely simple operation. In addition, the resin foam obtained by this method has good mechanical strength and low specific gravity, and because of its special foam structure, it can be used for special applications such as diaphragms such as speakers and microphones. it can.
【図１】 本発明の製法における樹脂体の不活性ガス含
浸量の濃度勾配の例を示すグラフである。FIG. 1 is a graph showing an example of a concentration gradient of an amount of an inert gas impregnated in a resin body in a production method of the present invention.
【図２】 図１に示す濃度勾配を有する樹脂体を加熱、
発泡させた樹脂発泡体の断面構造を模式的に示す断面図
である。2 heats a resin body having a concentration gradient shown in FIG. 1,
FIG. 3 is a cross-sectional view schematically illustrating a cross-sectional structure of a foamed resin foam.
【図３】 本発明の製法における樹脂体の不活性ガス含
浸量の濃度勾配の他の例を示すグラフである。FIG. 3 is a graph showing another example of the concentration gradient of the amount of inert gas impregnated in the resin body in the production method of the present invention.
【図４】 図２に示す濃度勾配を有する樹脂体を加熱発
泡させた樹脂発泡体の断面図を模式的に示す断面図であ
る。FIG. 4 is a cross-sectional view schematically showing a cross-sectional view of a resin foam obtained by heating and foaming a resin body having a concentration gradient shown in FIG.
【図５】 実施例１で得られた発泡シートの断面の発泡
構造を示す顕微鏡写真である。FIG. 5 is a micrograph showing a foam structure of a cross section of the foam sheet obtained in Example 1.
【図６】 実施例２で得られた発泡シートの断面の発泡
構造を示す顕微鏡写真である。FIG. 6 is a photomicrograph showing a foam structure of a cross section of the foam sheet obtained in Example 2.
Claims (1)
厚み方向に不活性ガスの含浸量の濃度勾配を形成し、つ
いでこれを加熱して樹脂体を発泡させることを特徴とす
る樹脂発泡体の製法。1. A resin body is impregnated with an inert gas, a concentration gradient of the amount of the inert gas impregnated in the thickness direction of the resin body is formed, and then the resin body is heated to foam the resin body. Manufacturing method of resin foam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26769397A JP4178567B2 (en) | 1997-09-12 | 1997-09-12 | Production method of resin foam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26769397A JP4178567B2 (en) | 1997-09-12 | 1997-09-12 | Production method of resin foam |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH1180408A true JPH1180408A (en) | 1999-03-26 |
| JP4178567B2 JP4178567B2 (en) | 2008-11-12 |
Family
ID=17448232
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26769397A Expired - Fee Related JP4178567B2 (en) | 1997-09-12 | 1997-09-12 | Production method of resin foam |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4178567B2 (en) |
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