JP5205636B2 - Manufacturing method of resin structure - Google Patents
Manufacturing method of resin structure Download PDFInfo
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- JP5205636B2 JP5205636B2 JP2007076552A JP2007076552A JP5205636B2 JP 5205636 B2 JP5205636 B2 JP 5205636B2 JP 2007076552 A JP2007076552 A JP 2007076552A JP 2007076552 A JP2007076552 A JP 2007076552A JP 5205636 B2 JP5205636 B2 JP 5205636B2
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- carbon dioxide
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- 239000011347 resin Substances 0.000 title claims description 71
- 229920005989 resin Polymers 0.000 title claims description 71
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 72
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 36
- 239000001569 carbon dioxide Substances 0.000 claims description 36
- 239000007787 solid Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 22
- 238000003466 welding Methods 0.000 claims description 15
- 239000010419 fine particle Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 8
- 238000005187 foaming Methods 0.000 claims description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 5
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 5
- 230000009477 glass transition Effects 0.000 claims description 3
- 229920005992 thermoplastic resin Polymers 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 2
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 2
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229920005669 high impact polystyrene Polymers 0.000 description 2
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- 239000000843 powder Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
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- 229920002319 Poly(methyl acrylate) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- FGDAXMHZSNXUFJ-UHFFFAOYSA-N ethene;prop-1-ene;prop-2-enenitrile Chemical group C=C.CC=C.C=CC#N FGDAXMHZSNXUFJ-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 239000012467 final product Substances 0.000 description 1
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- 229910003475 inorganic filler Inorganic materials 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
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- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
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- 238000007747 plating Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000120 polyethyl acrylate Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Images
Description
近年、亜臨界状態または超臨界状態における流体の特異な性質が注目され、それを利用した応用が進んでいる。
中でも二酸化炭素は、化学的に不活性で安全であるという特徴のため、種種の利用が図られている。二酸化炭素は無毒性のガスであり、加圧下で熱可塑性樹脂にとけ込む一方、常温常圧では樹脂に少量しか溶解しないという特徴を有する。さらに、二酸化炭素は３１．０℃、７．４ＭＰａ以上と比較的温和な条件において超臨界状態になり、各種の機能を発現するという特徴を有している。
具体的には、亜臨界状態または超臨界状態の二酸化炭素を溶媒として利用する方法として、反応場としての利用、物質の抽出・分離に際しての利用、溶解させた物質を析出させて微粒子を作るための利用等が提案されている。さらに、亜臨界状態または超臨界状態の二酸化炭素を溶質として利用する方法として、繊維染色、表面メッキ、高分子ブレンド、微細発泡への利用が提案されている。
しかし、亜臨界状態または超臨界状態の流体の特性を利用して、固体樹脂同士を溶着する方法は知られていなかった。
また、高分子多孔体を形成する方法としては、高分子に二酸化炭素を加圧して溶解させ、その後減圧または昇温操作を行うことによって二酸化炭素が溶解できない状態とし、相変化を起こして気泡を樹脂中に発生させる方法が提案されていた。この方法から容易に理解できるように、得られる発泡体中の気泡は独立気泡となる。このような成形物は軽量化、および寸法安定性が望まれる用途には好適であるが、たとえば、フィルターや、タンパク質培養のための保持体のような連続気泡を有する発泡体が必要とされる用途には使用できなかった。
Of these, carbon dioxide is used in various ways because of its chemically inert and safe characteristics. Carbon dioxide is a non-toxic gas and has the characteristic that it dissolves in a thermoplastic resin under pressure while it dissolves in a small amount in the resin at room temperature and normal pressure. Further, carbon dioxide is characterized by being in a supercritical state under relatively mild conditions of 31.0 ° C. and 7.4 MPa or more and exhibiting various functions.
Specifically, as a method of using carbon dioxide in a subcritical state or supercritical state as a solvent, it is used as a reaction field, used for extraction / separation of substances, to precipitate fine particles by dissolving dissolved substances. The use of is proposed. Furthermore, as a method of using carbon dioxide in a subcritical state or supercritical state as a solute, use for fiber dyeing, surface plating, polymer blending, and fine foaming has been proposed.
However, a method for welding solid resins to each other by utilizing the characteristics of a fluid in a subcritical state or a supercritical state has not been known.
In addition, as a method of forming a polymer porous body, carbon dioxide is pressurized and dissolved in the polymer, and then the pressure is reduced or the temperature is raised to make the carbon dioxide insoluble. A method of generating in the resin has been proposed. As can be easily understood from this method, the bubbles in the obtained foam are closed cells. Such molded articles are suitable for applications where weight reduction and dimensional stability are desired, but for example, foams having open cells such as filters and holders for protein culture are required. It could not be used for the purpose.
本発明は亜臨界状態または超臨界状態の二酸化炭素を利用して固体樹脂同士を溶着する方法の提供、およびかかる方法を利用した連続気泡を有する構造物の製造方法の提供を目的とする。 An object of the present invention is to provide a method for welding solid resins together using carbon dioxide in a subcritical state or a supercritical state, and a method for producing a structure having open cells using such a method.
本発明は、固体樹脂が配置された容器内に二酸化炭素を導入する工程、
前記二酸化炭素を亜臨界状態または超臨界状態にする工程、
上記の条件下で保持し、固体樹脂を溶着する工程、および
亜臨界状態または超臨界状態を解除する工程を含む、樹脂構造物の製造方法を提供する。
固体樹脂とは任意の形状の固体の樹脂をいい、たとえば、微粒子またはシートであることができる。
二酸化炭素を亜臨界状態または超臨界状態にするとは、二酸化炭素を前記のように３１．０℃、７．４ＭＰａ以上の条件下において超臨界状態とするか、または臨界温度よりわずかに低い温度領域での高密度状態である亜臨界状態とすることをいう。より具体的には、０℃から１００℃までの温度範囲、１から３０ＭＰａの圧力範囲内の二酸化炭素を使用できる。
溶着とは、固体樹脂同士が互いにその接触面において一体となり、強固に結合されることをいう。
亜臨界状態または超臨界状態を解除するとは、亜臨界状態または超臨界状態から通常の状態に戻すことをいい、たとえば、減圧または冷却により、亜臨界状態または超臨界状態を解消することをいう。
樹脂構造物とは、溶着された複数の固体樹脂により形成されるものをいう。
本発明の特定の態様においては、溶着点に対して圧力が加えられることができる。
本発明により得られる樹脂構造物は、その内部に気泡を有しないものであることができるし、異なる態様においては、その内部に気泡を有することができる。
The present invention includes a step of introducing carbon dioxide into a container in which a solid resin is disposed,
Bringing the carbon dioxide into a subcritical or supercritical state;
Provided is a method for producing a resin structure, which includes a step of holding a solid resin under the above-described conditions and a step of releasing a subcritical state or a supercritical state.
The solid resin refers to a solid resin having an arbitrary shape, and may be, for example, a fine particle or a sheet.
To make carbon dioxide into a subcritical state or a supercritical state, the carbon dioxide is brought into a supercritical state under the conditions of 31.0 ° C. and 7.4 MPa or more as described above, or a temperature range slightly lower than the critical temperature. The subcritical state, which is a high density state in More specifically, carbon dioxide within a temperature range of 0 ° C. to 100 ° C. and a pressure range of 1 to 30 MPa can be used.
Welding means that solid resins are integrated with each other at their contact surfaces and are firmly bonded.
Canceling the subcritical state or supercritical state means returning from the subcritical state or supercritical state to the normal state, for example, eliminating the subcritical state or supercritical state by reducing the pressure or cooling.
The resin structure means one formed by a plurality of welded solid resins.
In a particular embodiment of the invention, pressure can be applied to the welding point.
The resin structure obtained by the present invention can have no air bubbles inside thereof, and in a different embodiment, it can have air bubbles inside thereof.
本発明の効果は、亜臨界状態または超臨界状態において二酸化炭素をポリマー中に溶解させることにより生ずる、ガラス転移点の低下及び粘度の低下現象に起因するものと考えられる。これはプラスチックの分子鎖間の相互作用が溶解ガスによって低下し高分子鎖の移動度が上がるためと言われている。樹脂に対するガスの溶解度が上昇すると粘度低下がより進行するという報告もある。また含浸の特徴として、ヘンリー定数に比例して圧力が上昇すると共に樹脂へのガス溶解度が比例して増加すると言われている。すなわち、圧力を増加させると樹脂に対する溶解度が増加し、粘度が大きく低下することとなる。よって、二酸化炭素ガスは圧力７ＭＰａ以下の領域でも、温度３１℃以下の領域でも、樹脂への溶解が可能である。なお、温度が低いほど樹脂に対するガスの溶解度は高い。 The effect of the present invention is considered to be caused by a phenomenon of a decrease in glass transition point and a decrease in viscosity caused by dissolving carbon dioxide in a polymer in a subcritical state or a supercritical state. This is said to be because the interaction between plastic molecular chains is lowered by the dissolved gas and the mobility of the polymer chains is increased. There is also a report that the viscosity lowers more as the solubility of the gas in the resin increases. Further, as a characteristic of impregnation, it is said that the pressure increases in proportion to the Henry constant and the gas solubility in the resin increases in proportion. That is, when the pressure is increased, the solubility in the resin is increased and the viscosity is greatly reduced. Therefore, carbon dioxide gas can be dissolved in the resin even in a region where the pressure is 7 MPa or less and in a region where the temperature is 31 ° C. or less. In addition, the solubility of the gas with respect to resin is so high that temperature is low.
上記のシステムにより樹脂内部に二酸化炭素が進入して、粘度が低下された樹脂では、隣接する固体樹脂の表層同士が一体となり、両者はその境界面で融合する。その後の亜臨界状態または超臨界状態の解除により、固体樹脂の状態が固定されたまま二酸化炭素が除去され、固体樹脂同士が強固に結合されるものと考えられている。 In the resin whose viscosity is lowered by carbon dioxide entering the resin by the above system, the surface layers of adjacent solid resins are integrated with each other, and both fuse at the boundary surface. Subsequent cancellation of the subcritical state or supercritical state is considered to remove carbon dioxide while the state of the solid resin is fixed, so that the solid resins are firmly bonded to each other.
本発明により、固体樹脂を溶着して樹脂構造物を成形するための新規な製造方法が提供される。本発明の方法では、粘度のコントロールは亜臨界状態または超臨界二酸化炭素による含浸での粘度低下により行うため、熱の出入りが少なく、温度勾配、熱の出入りのコントロールをせずに成形できるという利点を有する。
また、本発明の方法では荷重をかけずに形成できるため、得られた構造物内の残留応力が無い。そのためたとえば、微粒子の樹脂固体を薄く配置して成形することにより良好な光学特性を有するフィルムを成形することも可能である。
The present invention provides a novel production method for forming a resin structure by welding a solid resin. In the method of the present invention, the viscosity is controlled by lowering the viscosity in the subcritical state or impregnation with supercritical carbon dioxide, so that there is little heat in / out and molding can be performed without controlling the temperature gradient and heat in / out. Have
Moreover, since it can form without applying a load in the method of this invention, there is no residual stress in the obtained structure. Therefore, for example, it is also possible to form a film having good optical characteristics by thinly arranging resin solids of fine particles.
本発明の方法において樹脂の微粒子を固体樹脂として使用して、微粒子同士を結合することにより、粒子の間に空隙が形成された多孔質の部材を形成することができる。この空隙は連続気泡として機能し、フィルターやタンパク質培養のための保持体として良好な特性を付与する。この場合には粒径を選択することにより空隙の大きさを制御することができるので、フィルターとして使用する場合の性能制御が容易となる。たとえば、水を通さずに蒸気だけを通すフィルターなどの用途が期待される。
またタンパク質の培養に関しては、タンパク質に酸素や、栄養分を多く送り込む必要性から、比表面積が非常に大きい微細多孔体が望まれているので、微粒子の粒径を選択することにより簡単に比表面積を調節できる本発明の方法は非常に有用である。
また、二酸化炭素を使用するので、有害物を排出せず、成形コストが低く、安全な樹脂構造物の製造方法が提供される。また低温度での成形が可能なため、タンパク質培養のための保持体を製造する場合には、生物を培養させたまま成形することが可能となる。
In the method of the present invention, by using fine particles of resin as a solid resin and bonding the fine particles, a porous member having voids formed between the particles can be formed. This void functions as an open cell and gives good properties as a support for a filter or protein culture. In this case, the size of the void can be controlled by selecting the particle size, so that the performance control when used as a filter becomes easy. For example, applications such as a filter that allows only steam to pass without passing water are expected.
In addition, regarding protein culture, a microporous material with a very large specific surface area is desired because of the need to send oxygen and nutrients to the protein, so the specific surface area can be easily set by selecting the particle size of the fine particles. The method of the present invention that can be adjusted is very useful.
In addition, since carbon dioxide is used, there is provided a safe method for producing a resin structure that does not discharge harmful substances, has low molding costs. In addition, since molding at a low temperature is possible, when producing a holding body for protein culture, it is possible to mold the organism while culturing it.
本発明における操作をより詳細に以下に説明する。
本発明の固体樹脂が配置された容器内に二酸化炭素を導入する工程では、固体樹脂を容器内に置き、その後二酸化炭素を容器内に導入する。固体樹脂の配置はたとえば、樹脂の粉末やペレットなどを充填することにより行うことができる。また粒子状の固体を媒体中に分散し、これを容器内に投入した後、分散媒を蒸発などにより除去することにより、樹脂を配置することもできる。一般に、容器は最終製品の形状に対応して選択することができる。
前記二酸化炭素を亜臨界状態または超臨界状態にする工程では、上記の容器を密閉し、導入した二酸化炭素が亜臨界状態または超臨界状態となる条件に加熱および／または加圧する。加熱方法および加圧方法としては任意の方法が使用できるが、加熱速度、加圧速度を正確に制御することが好ましい。
上記の条件下で保持し、固体樹脂を溶着する工程では、前記の状態に十分な時間保持し、固体樹脂同士を互いに結合させる。この際、温度および圧力を調節することにより、溶着の状態を制御することができる。この条件は使用する樹脂の種類によって変化するが、一般的には温度は０℃から１００℃の範囲、圧力は１から３０ＭＰａの範囲であり、保持時間は約１−２４時間である。この条件範囲は、後述の実施例において使用されるポリメチルメタアクリレートの場合にも当てはまる。また処理温度は樹脂のガラス転移温度または融点よりも低い温度とされるべきである。
The operation in the present invention will be described in more detail below.
In the step of introducing carbon dioxide into the container in which the solid resin of the present invention is disposed, the solid resin is placed in the container, and then carbon dioxide is introduced into the container. The arrangement of the solid resin can be performed, for example, by filling resin powder or pellets. Alternatively, the resin can be disposed by dispersing the particulate solid in a medium, putting it in a container, and then removing the dispersion medium by evaporation or the like. In general, the container can be selected according to the shape of the final product.
In the step of bringing the carbon dioxide into a subcritical state or a supercritical state, the container is sealed, and the introduced carbon dioxide is heated and / or pressurized to a condition that makes the subcritical state or the supercritical state. Although any method can be used as the heating method and the pressurizing method, it is preferable to accurately control the heating rate and the pressurizing rate.
In the step of holding under the above-described conditions and welding the solid resin, the solid resin is held in the above state for a sufficient time to bond the solid resins together. At this time, the welding state can be controlled by adjusting the temperature and pressure. This condition varies depending on the type of resin used, but generally the temperature is in the range of 0 ° C. to 100 ° C., the pressure is in the range of 1 to 30 MPa, and the holding time is about 1-24 hours. This condition range also applies to the case of polymethyl methacrylate used in the examples described later. The treatment temperature should be lower than the glass transition temperature or melting point of the resin.
亜臨界状態または超臨界状態を解除する工程では、冷却および／または減圧により流体を亜臨界状態または超臨界状態から戻す。冷却速度および減圧速度も、固体樹脂の組成などにより変化するが、具体的な条件は実験により適宜決定することができる。一般的には、冷却速度は０．００１℃／秒から３０℃／秒、減圧速度は０．０５ＭＰａ／分から１０ＭＰａ／分の範囲である。この条件範囲は、後述の実施例において使用されるポリメチルメタアクリレートの場合にも当てはまる。 In the step of releasing the subcritical state or the supercritical state, the fluid is returned from the subcritical state or the supercritical state by cooling and / or decompression. Although the cooling rate and the reduced pressure rate also vary depending on the composition of the solid resin and the like, specific conditions can be appropriately determined by experiment. In general, the cooling rate is in the range of 0.001 ° C./second to 30 ° C./second, and the pressure reduction rate is in the range of 0.05 MPa / minute to 10 MPa / minute. This condition range also applies to the case of polymethyl methacrylate used in the examples described later.
先の溶着工程での保持時間と、亜臨界状態または超臨界状態の解除工程での冷却および／または減圧の速度により、得られる樹脂構造物の発泡状態を制御することができる。すなわち、保持時間が長いほど樹脂固体の内部まで二酸化炭素が含浸され、亜臨界状態または超臨界状態を解除する際に発泡が起こりやすくなる。したがって、発泡体が望まれる場合には保持時間を長くすることが好ましい。二酸化炭素を除去する際に、減圧を急速に行ったり、減圧により亜臨界状態または超臨界状態を脱した後に昇温することにより、発泡させることもできる。発泡により構造物の軽量化が図れる他、樹脂固体の溶着点に圧力が加えられるため、構造物の強度を上げることができる。 The foamed state of the resulting resin structure can be controlled by the holding time in the previous welding step and the cooling and / or pressure reduction rate in the subcritical state or supercritical state releasing step. That is, as the holding time is longer, carbon dioxide is impregnated into the resin solid, and foaming is likely to occur when the subcritical state or the supercritical state is released. Therefore, if a foam is desired, it is preferable to increase the holding time. When removing carbon dioxide, foaming can also be performed by rapidly reducing the pressure, or by raising the temperature after removing the subcritical or supercritical state by reducing the pressure. In addition to reducing the weight of the structure by foaming, pressure is applied to the welding point of the resin solid, so that the strength of the structure can be increased.
樹脂としては、亜臨界状態または超臨界状態の二酸化炭素で粘度を低下することのできる任意の樹脂が使用できるが、一般的には熱可塑性樹脂が使用され、典型的にはポリエチレン、ポリプロピレンなどのポリオレフィン樹脂、塩化ビニル樹脂などの塩素化ポリオレフィン、ポリメチルアクリレート、ポリエチルアクリレート、ポリメチルメタアクリレートなどのポリアクリレートおよびポリメタアクリレート、酢酸ビニルやＥＶＡなどのビニル樹脂、および耐衝撃性ポリスチレン（ＨＩＰＳ）、アクリロニトリルブタジエンスチレン樹脂（ＡＢＳ）、アクリロニトリル−エチレンプロピレンゴム−スチレン樹脂（ＡＥＳ）などの複合樹脂を使用することができる。しかし、たとえば、熱硬化性の樹脂であっても、架橋度が低く、その表層の粘度が超臨界流体により低下される場合には使用することができる。また、硬化前の樹脂またはＢ−ステージ状態の樹脂を使用して構造物を形成した後に、樹脂を硬化することもできる。
また、たとえば、カーボン粒子、金属粉、顔料、炭酸カルシウムなどの無機充填剤、ガラス繊維などの各種繊維、ナノファイバー、カーボナノチューブ、ウイスカーなどの強化材を樹脂に混合することもできる。
As the resin, any resin that can be reduced in viscosity by subcritical or supercritical carbon dioxide can be used, but generally a thermoplastic resin is used, typically polyethylene, polypropylene, etc. Polychlorinated resins such as polyolefin resins and vinyl chloride resins, polyacrylates and polymethacrylates such as polymethyl acrylate, polyethyl acrylate and polymethyl methacrylate, vinyl resins such as vinyl acetate and EVA, and high impact polystyrene (HIPS) Composite resins such as acrylonitrile butadiene styrene resin (ABS) and acrylonitrile-ethylene propylene rubber-styrene resin (AES) can be used. However, for example, even a thermosetting resin can be used when the degree of crosslinking is low and the viscosity of the surface layer is lowered by the supercritical fluid. Moreover, after forming a structure using resin before hardening or resin of a B-stage state, resin can also be hardened.
In addition, for example, carbon particles, metal powder, pigments, inorganic fillers such as calcium carbonate, various fibers such as glass fibers, and reinforcing materials such as nanofibers, carbon nanotubes, and whiskers can be mixed into the resin.
実施例
材料はポリメチルメタクリレート（旭化成ケミカルズ株式会社 デルペット５６０Ｆ）（Ｔｇ１０１℃（実測値）メルトフローレイト１３．０ｇ／１０分）（カタログ値））の高さ３．２ｍｍ、直径２．５５ｍｍの円筒状のペレット）を使用した。
高圧ガス容器内を３０℃にした後、図１に示すように、上記の試料を金属製の皿に乗せ容器に挿入した。その後二酸化炭素を導入し、容器内温度３０℃、容器内圧力８ＭＰａに、３時間保持して、試験片に二酸化炭素を含浸させた。その後０．５ＭＰａ／分の減圧速度で減圧し、試料を取り出した。成形後の全体像を図２に示す。図３には試料の溶着点の拡大図を示す。試料同士が溶着していることを確認した。また内部が発泡していることも確認した。
Example Material is polymethyl methacrylate (Asahi Kasei Chemicals Corporation Delpet 560F) (Tg 101 ° C. (actual value) melt flow rate 13.0 g / 10 min) (catalog value) height 3.2 mm, diameter 2.55 mm Cylindrical pellets) were used.
After setting the inside of the high-pressure gas container to 30 ° C., as shown in FIG. 1, the sample was placed on a metal dish and inserted into the container. Thereafter, carbon dioxide was introduced, and the test piece was impregnated with carbon dioxide at a temperature in the container of 30 ° C. and a pressure in the container of 8 MPa for 3 hours. Thereafter, the pressure was reduced at a pressure reduction rate of 0.5 MPa / min, and the sample was taken out. The overall image after molding is shown in FIG. FIG. 3 shows an enlarged view of the welding point of the sample. It was confirmed that the samples were welded together. It was also confirmed that the inside was foamed.
Claims (9)
前記二酸化炭素を亜臨界状態または超臨界状態にする工程、
上記の条件下で保持し、固体樹脂を溶着する工程、および
亜臨界状態または超臨界状態を解除する工程を含む、
粒子の間に連続気泡として空隙が形成されたフィルターの製造方法。 Introducing carbon dioxide into a container in which fine particles of a solid resin are disposed;
Bringing the carbon dioxide into a subcritical or supercritical state;
Holding under the above conditions, welding a solid resin, and releasing the subcritical or supercritical state,
A method for producing a filter in which voids are formed as open cells between particles.
前記二酸化炭素を亜臨界状態または超臨界状態にする工程、
上記の条件下で保持し、固体樹脂を溶着する工程、および
亜臨界状態または超臨界状態を解除する工程を含む、
粒子の間に連続気泡として空隙が形成された生物培養のための保持体の製造方法。 Introducing carbon dioxide into a container in which fine particles of a solid resin are disposed;
Bringing the carbon dioxide into a subcritical or supercritical state;
Holding under the above conditions, welding a solid resin, and releasing the subcritical or supercritical state,
A method for producing a holder for biological culture in which voids are formed as open cells between particles.
前記二酸化炭素を亜臨界状態または超臨界状態にする工程、
上記の条件下で保持し、固体樹脂を溶着する工程、および
亜臨界状態または超臨界状態を解除する工程を含む方法により製造された、粒子の間に形成された空隙が連続気泡として作用するフィルター。 Introducing carbon dioxide into a container in which fine particles of a solid resin are disposed;
Bringing the carbon dioxide into a subcritical or supercritical state;
A filter produced by a method comprising a step of maintaining a solid resin and holding a solid resin, and a step of releasing a subcritical or supercritical state, wherein voids formed between particles act as open cells. .
前記二酸化炭素を亜臨界状態または超臨界状態にする工程、
上記の条件下で保持し、固体樹脂を溶着する工程、および
亜臨界状態または超臨界状態を解除する工程を含む方法により製造された、粒子の間に形成された空隙が連続気泡として作用する生物培養のための保持体。 Introducing carbon dioxide into a container in which fine particles of a solid resin are disposed;
Bringing the carbon dioxide into a subcritical or supercritical state;
A living body in which voids formed between particles act as open cells, which are produced by a method comprising the steps of holding a solid resin and holding the solid resin, and releasing the subcritical or supercritical state. Holder for culture.
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