JP4344216B2 - Method for producing porous polymer compound having open cells - Google Patents
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Description
本発明は、連続気泡を有する高分子化合物多孔体の製造方法に関するものである。 The present invention relates to a method for producing a polymer compound porous body having open cells.
連続気泡を有する高分子化合物多孔体は、主にインク内蔵タイプの印判に用いられてきた。 High molecular compound porous bodies having open cells have been mainly used for ink-embedded type seals.
従来、連続気泡を有する高分子化合物多孔体は、高分子化合物と溶媒溶解性の微粉末を、ニーダー等で加熱混合し、溶媒溶解性の微粉末を溶媒により溶解除去して製造されていた。 Conventionally, a polymer compound porous body having open cells has been produced by heating and mixing a polymer compound and a solvent-soluble fine powder with a kneader or the like, and dissolving and removing the solvent-soluble fine powder with a solvent.
例えば、特許文献１には、熱可塑性樹脂粉末基材に合成ゴム溶液を混和して乾燥させたものに、界面活性剤粉末と塩化ナトリウム等の易水溶性塩微粉末を混和し成形した後、界面活性剤粉末と易水溶性塩微粉末を洗除する方法が記載されている。 For example, in Patent Document 1, after a synthetic rubber solution is mixed with a thermoplastic resin powder base material and dried, a surfactant powder and a water-soluble salt fine powder such as sodium chloride are mixed and molded, A method for washing the surfactant powder and the finely water-soluble salt fine powder is described.
また、特許文献２には、ポリオレフィン樹脂とポリオレフィン樹脂より高い融点を有する塩化ナトリウム等の水易溶性微粉末と水溶性有機化合物を混練した後シート状に成形してシート体とし、シート体に含有される水易溶解性微粉末と水溶性有機化合物を除去して多孔性シートとし、多孔性シートを加圧圧縮して気泡を縮小させたポリオレフィン多孔体が記載されている。 Patent Document 2 discloses that a polyolefin resin and a water-soluble organic compound such as sodium chloride having a melting point higher than that of the polyolefin resin and a water-soluble organic compound are kneaded and then formed into a sheet to form a sheet, which is contained in the sheet There is described a polyolefin porous body in which a readily water-soluble fine powder and a water-soluble organic compound are removed to form a porous sheet, and the porous sheet is compressed and compressed to reduce bubbles.
しかしながら、特許文献１および特許文献２に開示された方法では、樹脂の深部に存在する微粉末を抽出除去するには技術を要した。 However, the methods disclosed in Patent Document 1 and Patent Document 2 require a technique for extracting and removing fine powders existing in the deep part of the resin.
さらに、特許文献３には、ポリオレフィン系樹脂に特定粒径の亜硫酸カルシウムおよび／または硫酸カルシウムからなる無機塩を添加した混合物を押出法によってシート状に成形し、この成形物を無機塩を溶解しうる無機酸で処理した後アルカリで中和することを特徴とする多孔性ポリオレフィン系樹脂シートの製造法が記載されている。 Further, in Patent Document 3, a mixture obtained by adding an inorganic salt composed of calcium sulfite and / or calcium sulfate having a specific particle diameter to a polyolefin resin is molded into a sheet by an extrusion method, and the molded product is dissolved in an inorganic salt. A method for producing a porous polyolefin-based resin sheet is described, which is characterized by neutralizing with an alkali after being treated with an inorganic acid.
特許文献３に記載された方法は、無機塩を溶解するために無機酸を使用しなければならず、耐食性の装置を用いなければならないという難点があった。 The method described in Patent Document 3 has a drawback in that an inorganic acid must be used to dissolve the inorganic salt, and a corrosion-resistant device must be used.
さらに、また特許文献１〜特許文献３に記載された従来技術は、いずれも無機塩を溶解除去するには時間を要し、生産性が低いものであった。
本発明が解決しようとする課題は、耐食性の製造装置を必要とせず、効率的に連続気泡を有する多孔質の高分子化合物を製造する方法を提供することである。 The problem to be solved by the present invention is to provide a method for efficiently producing a porous polymer compound having open cells without requiring a corrosion-resistant production apparatus.
本発明者らは鋭意研究を重ねた結果、高分子化合物を有機溶剤に溶解させ、特定の微粉末を加え微粉末を溶解除去することにより、上記課題を解決できることを見出し、本発明を完成するに至った。 As a result of intensive studies, the present inventors have found that the above-mentioned problems can be solved by dissolving a polymer compound in an organic solvent, adding a specific fine powder, and dissolving and removing the fine powder, thereby completing the present invention. It came to.
すなわち、本発明は、高分子化合物は溶解するが糖類は溶解しない有機溶剤に高分子化合物と微粉末の糖類を加えて糖類含有高分子化合物溶液を調製した後、該糖類含有高分子化合物溶液から有機溶剤を除去して糖類含有高分子化合物を調製し、該糖類含有高分子化合物から微粉末の糖類を除去することを特徴とする連続気泡を有する高分子化合物多孔体の製造方法に関するものである。 That is, the present invention prepares a saccharide-containing polymer compound solution by adding a polymer compound and fine saccharides to an organic solvent in which the polymer compound dissolves but does not dissolve saccharides. The present invention relates to a method for producing a porous polymer compound having open cells, characterized in that an organic solvent is removed to prepare a saccharide-containing polymer compound, and fine powdered saccharide is removed from the saccharide-containing polymer compound. .
本発明は、気泡体を形成するための分粉末物質として糖類を用いるため、糖類を除去する溶剤は水でよいため、耐食性の製造装置を必要としない。また、無機塩を用いた場合に比べて、糖類を溶解除去する時間が短いため、生産性が向上する。また、高分子化合物を有機溶剤で溶解するだけでよく、従来技術のように高分子化合物を加熱成形する必要がないため、本発明方法の高分子物質多孔体の製造に要するエネルギーはより少なくなる。さらに、また本発明で得られた高分子化合物多孔体は、水は透過しないが、気体は透過する性質を有している。 In the present invention, since saccharides are used as a powdered substance for forming bubbles, the solvent for removing the saccharides may be water, so that a corrosion-resistant manufacturing apparatus is not required. Moreover, since the time for dissolving and removing the saccharide is shorter than in the case of using an inorganic salt, productivity is improved. In addition, since it is only necessary to dissolve the polymer compound in an organic solvent and it is not necessary to heat mold the polymer compound as in the prior art, less energy is required to produce the porous polymer material of the method of the present invention. . Furthermore, the polymer compound porous body obtained by the present invention has a property of not allowing water to permeate but allowing gas to permeate.
本発明は、有機溶剤に高分子化合物を溶解した高分子化合物溶液に、微粉末の糖類を加えた後、有機溶剤と糖類を除去することにより、連続気泡を有する高分子化合物多孔体を製造することを特徴とするものである。 The present invention produces a polymer compound porous body having open cells by adding a fine powder of saccharide to a polymer compound solution obtained by dissolving a polymer compound in an organic solvent, and then removing the organic solvent and the saccharide. It is characterized by this.
本発明の高分子化合物多孔体の基材となる高分子化合物は、後述する有機溶剤に可溶であればよい。そのような高分子化合物としては、例えばスチレン系エラストマーやオレフィン系エラストマー等の熱可塑性エラストマー、ＮＲ、ＳＢＲ、ＥＰＤＭ、含ハロゲンゴム等のゴム、ＰＥ、ＰＰ、ＰＳ、塩化ビニル等のプラスチックを挙げることができる。これらの高分子化合物のなかでも、加硫工程を必要としない点、弾性、リサイクル性の点で、熱可塑性エラストマーが好ましい。 The high molecular compound used as the base material of the high molecular compound porous body of the present invention may be soluble in the organic solvent described later. Examples of such polymer compounds include thermoplastic elastomers such as styrene elastomers and olefin elastomers, rubbers such as NR, SBR, EPDM, and halogen-containing rubbers, and plastics such as PE, PP, PS, and vinyl chloride. Can do. Among these polymer compounds, a thermoplastic elastomer is preferable from the viewpoint of not requiring a vulcanization step, elasticity and recyclability.
本発明で用いられる有機溶剤は、上記高分子化合物を溶解し、糖類を溶解することのない有機溶剤であればよい。そのような有機溶剤としては、例えばキシレン、ＤＭＦ、ゴム揮、ＭＥＫ、酢酸エチル等を挙げることができる。これらの有機溶剤のなかでも、匂い、沸点、溶解力の点で、キシレンが好ましい。 The organic solvent used in the present invention may be any organic solvent that dissolves the polymer compound and does not dissolve saccharides. Examples of such an organic solvent include xylene, DMF, rubber volatilization, MEK, and ethyl acetate. Among these organic solvents, xylene is preferable in terms of odor, boiling point, and dissolving power.
本発明における、高分子化合物多孔体の製造方法の製造方法の一実施形態としては以下の方法が挙げられる。 The following method is mentioned as one Embodiment of the manufacturing method of the manufacturing method of a polymeric compound porous body in this invention.
まず、上記有機溶剤に上記高分子化合物を溶解させる。溶解方法は、特に限定されるものではなく、有機溶剤に粉末状の高分子化合物を加えて、攪拌混合すればよい。有機溶剤の量は、基材となる高分子化合物の種類によって異なるが、高分子化合物を溶解できる程度の量であればよい。例えば、熱可塑性エラストマーの場合、熱可塑性エラストマー１００ｇ当たり、有機溶剤を１００〜１０００ｍｌ用いればよい。 First, the polymer compound is dissolved in the organic solvent. The dissolution method is not particularly limited, and a powdery polymer compound may be added to an organic solvent and mixed with stirring. The amount of the organic solvent varies depending on the type of the polymer compound serving as the base material, but may be an amount that can dissolve the polymer compound. For example, in the case of a thermoplastic elastomer, 100 to 1000 ml of an organic solvent may be used per 100 g of the thermoplastic elastomer.
高分子化合物溶液を調製するに際し、増量や非粘着等の目的で、炭酸カルシウム、クレー、シリカ等の無機充填材を添加したり、分散性と離型性を向上させる目的で、ステアリン酸やステアリン酸塩類等の高級脂肪酸化合物を添加してもよい。 When preparing a polymer compound solution, an inorganic filler such as calcium carbonate, clay or silica is added for the purpose of increasing the amount or non-adhesion, and stearic acid or stearin is used for the purpose of improving dispersibility and mold release. Higher fatty acid compounds such as acid salts may be added.
得られた高分子化合物溶液に、微粉末の糖類を加えて、糖類含有高分子化合物溶液を調製する。糖類を溶解しない有機溶剤を用いるため、糖類含有高分子溶液中では、糖類が微粉末のまま懸濁した状態で存在する。本発明に用いる糖類としては、フルクトース、グルコース等の単糖類、スクロース等の二糖類、でんぷん等の多糖類等の糖類を挙げることができるが、抽出溶解性、融点、価格等の理由によりスクロースが好ましい。 A saccharide-containing polymer compound solution is prepared by adding fine powdered saccharides to the polymer compound solution obtained. Since an organic solvent that does not dissolve saccharides is used, the saccharides are present in a suspended state in a fine powder in the saccharide-containing polymer solution. Examples of the saccharides used in the present invention include monosaccharides such as fructose and glucose, disaccharides such as sucrose, and saccharides such as polysaccharides such as starch, but sucrose is used for reasons such as extraction solubility, melting point, and price. preferable.
これらの糖類は、粒径が１ｍｍ〜３０μｍ、好ましくは、０．５ｍｍ〜５０μｍの微粉末のものが、強度及び柔軟性の点で好ましい。 These saccharides are preferably fine powders having a particle size of 1 mm to 30 μm, preferably 0.5 mm to 50 μm from the viewpoint of strength and flexibility.
次いで、糖類含有高分子化合物溶液から有機溶剤を除去して糖類含有高分子化合物を調製する。有機溶剤を除去する方法は、特に限定されないが、常圧下または減圧下で溶剤を除去して、糖類含有高分子化合物を調製すればよい。 Next, the organic solvent is removed from the saccharide-containing polymer compound solution to prepare a saccharide-containing polymer compound. The method for removing the organic solvent is not particularly limited, and the saccharide-containing polymer compound may be prepared by removing the solvent under normal pressure or reduced pressure.
得られた糖類含有高分子化合物から、糖類を除去することにより、連続気泡を有する高分子化合物多孔体が得られる。糖類を除去する手段としては、水を用いて糖類を溶解除去する手段が挙げられる。糖類は、容易に水に溶解し、また装置を腐食することもないので、効率的かつ低コストで高分子化合物多孔体を得ることができる。 By removing the saccharide from the obtained saccharide-containing polymer compound, a polymer compound porous body having open cells can be obtained. Examples of means for removing saccharides include means for dissolving and removing saccharides using water. Since the saccharide easily dissolves in water and does not corrode the apparatus, the polymer compound porous body can be obtained efficiently and at low cost.
糖類を抽出除去するための抽出温度は、例えば、１０〜１００℃、好ましくは、
２０〜６０℃の間で適宜選択すればよい。糖類は、水の温度が高くなるほど、溶解度が上昇するので、温水を用いて、糖類を抽出除去することが好ましい。
The extraction temperature for extracting and removing sugars is, for example, 10 to 100 ° C., preferably
What is necessary is just to select suitably between 20-60 degreeC. Since the solubility of saccharide increases as the temperature of water increases, it is preferable to extract and remove the saccharide using warm water.
高分子多孔体を成形するには、有機溶剤を含む糖類含有高分子化合物溶液の状態で任意の形状に成形すればよい。フィルム状やシート状の高分子化合物多孔体を得るには、例えば糖類含有高分子化合物溶液を平板の上に流し込んで、有機溶剤を除去した後、フィルム状またはシート状の成形体を平板から剥離すればよい。また、立体的な高分子化合物多孔体を得るには、型を糖類含有高分子化合物溶液に浸漬して型の表面を被覆して有機溶剤を除去するか、型に糖類含有高分子化合物を塗布もしくはスプレーして皮膜を形成し、有機溶剤を除去してもよい。成形後の糖類含有高分子化合物から糖類を除去することにより、所望の形状の連続気泡を有する高分子化合物多孔体を得ることができる。 In order to mold the polymer porous body, it may be molded into an arbitrary shape in the state of a saccharide-containing polymer compound solution containing an organic solvent. In order to obtain a film-like or sheet-like polymer compound porous body, for example, a saccharide-containing polymer compound solution is poured onto a flat plate to remove the organic solvent, and then the film-like or sheet-like molded product is peeled off from the flat plate. do it. In order to obtain a three-dimensional porous polymer compound, the mold is immersed in a saccharide-containing polymer compound solution to cover the mold surface to remove the organic solvent, or the saccharide-containing polymer compound is applied to the mold. Alternatively, the organic solvent may be removed by spraying to form a film. By removing saccharides from the saccharide-containing polymer compound after molding, a polymer compound porous body having open cells of a desired shape can be obtained.
上記の実施形態の他に、有機溶剤に高分子化合物と糖類を同時に加えて、糖類含有高分子化合物溶液を調製してもよい。 In addition to the above embodiment, a saccharide-containing polymer compound solution may be prepared by simultaneously adding a polymer compound and a saccharide to an organic solvent.
下記の配合に従って、高分子化合物組成物を調製した。 A polymer compound composition was prepared according to the following formulation.
配合
(1)スチレン系熱可塑性エラストマー１） 40g
(2)スチレン系熱可塑性エラストマー２） 20g
(3)炭酸カルシウム３） 20g
(4)ステアリン酸４） 2g
Formulation
(1) Styrenic thermoplastic elastomer 1) 40g
(2) Styrenic thermoplastic elastomer 2) 20g
(3) Calcium carbonate 3) 20g
(4) Stearic acid 4) 2g
注：
１）JSR（株）製、商品名「SIS5229」
２）リケンテクノス（株）製、商品名「SEPS-3」
３）白石工業（株）製、商品名「シルバーＷ」
４）旭電化工業（株）製、商品名「SA-400」
note:
1) Product name "SIS5229", manufactured by JSR Corporation
2) Product name “SEPS-3”, manufactured by Riken Technos Co., Ltd.
3) Product name "Silver W", manufactured by Shiraishi Kogyo Co., Ltd.
4) Product name “SA-400” manufactured by Asahi Denka Kogyo Co., Ltd.
上記高分子化合物組成物を、500mlのビーカーに量り採り、キシレンを加えて400mlとし、溶解混合するまで攪拌して高分子化合物溶液を調製した。 The polymer compound composition was weighed into a 500 ml beaker, xylene was added to 400 ml, and the mixture was stirred until dissolved to prepare a polymer compound solution.
得られた高分子化合物溶液を200mlずつ500mlのビーカーに採り分けて、水溶性微粉末としてスクロース（日新製糖（株）製、商品名「フロストシュガー」）と塩化ナトリウム（和光純薬（株）製）を各々乳鉢で粉砕したものを、各々60g配合した。 The obtained polymer compound solution is separated into 200 ml beakers of 200 ml each, and sucrose (manufactured by Nissin Sugar Co., Ltd., trade name “Frost Sugar”) and sodium chloride (Wako Pure Chemical Industries, Ltd.) as water-soluble fine powders. 60 g of each crushed product in a mortar.
ガラスセル（90×110mm）に、上記水溶性微粉末含有高分子化合物溶液をそれぞれ約20mlづつ注ぎ入れ、乾燥してキシレンを除去し、セルから離型し、シート状サンプルを作った。 About 20 ml each of the above water-soluble fine powder-containing polymer compound solution was poured into a glass cell (90 × 110 mm), dried to remove xylene, and released from the cell to prepare a sheet-like sample.
シート状サンプルを長手方向に切り、45×110mmとして、500mlビーカーに水道水（20℃）を入れてサンプルを浸漬し、スクロースまたは食塩を抽出して高分子化合物多孔体を調製した。抽出速度を比較するために、浸漬後７時間と、２４時間後にそれぞれ乾燥して、抽出前後の重さを測定した。抽出用の水は、７時間までは、１時間おきに交換し、それ以降は放置した。スクロースを含む高分子化合物溶液から得たサンプルを実施例１とし、塩化ナトリウムを含む高分子化合物溶液から得たサンプルを比較例１として、水溶性物質の残留量を対比した。その結果を表１、表２に示す。 A sheet-like sample was cut in the longitudinal direction to obtain 45 × 110 mm, tap water (20 ° C.) was put into a 500 ml beaker, the sample was immersed, and sucrose or salt was extracted to prepare a polymer compound porous body. In order to compare the extraction speed, the sample was dried 7 hours after immersion and 24 hours after drying, and the weight before and after extraction was measured. The water for extraction was changed every 1 hour until 7 hours, and left after that. A sample obtained from a polymer compound solution containing sucrose was used as Example 1, and a sample obtained from a polymer compound solution containing sodium chloride was used as Comparative Example 1, and the residual amounts of water-soluble substances were compared. The results are shown in Tables 1 and 2.
残留量は、抽出前の水溶性微粉末の量を100%ととし、抽出後の高分子化合物多孔体に存在する水溶性微粉末の残量を％で表したものである。 The residual amount represents the remaining amount of the water-soluble fine powder existing in the polymer compound porous body after the extraction in terms of%, with the amount of the water-soluble fine powder before the extraction being 100%.
残留量を計算するための式を以下に示す。なお、式中の配合物総量とはキシレン以外の配合物（高分子化合物＋炭酸カルシウム＋ステアリン酸＋水溶性微粉末）の総量を表す。なお、計算値とは抽出前のサンプルのシートに含まれている水溶性微粉末の量（g）を示す。 The formula for calculating the residual amount is shown below. The total amount of the compound in the formula represents the total amount of the compound other than xylene (polymer compound + calcium carbonate + stearic acid + water-soluble fine powder). The calculated value indicates the amount (g) of the water-soluble fine powder contained in the sample sheet before extraction.
・計算値＝抽出前のサンプル重量（g）×水溶性微粉末（g）／配合物総量（g）
＝抽出前のサンプル重量（g）×60（g）／101（g）
＝抽出前のサンプル重量（g）×0.5941
・前後差＝抽出前のサンプル重量（g）−抽出後のサンプル重量（g）
・水溶性微粉末の抽出分（%）＝（前後差／計算値）×100
・残留量（%）＝100−抽出分（%）
-Calculated value = sample weight before extraction (g) x water-soluble fine powder (g) / total amount of compound (g)
= Sample weight before extraction (g) x 60 (g) / 101 (g)
= Sample weight before extraction (g) x 0.5941
-Difference before and after = sample weight before extraction (g)-sample weight after extraction (g)
-Extraction of water-soluble fine powder (%) = (front / back difference / calculated value) x 100
-Residual amount (%) = 100-Extraction (%)
表１および表２に示した結果から明らかなように、水溶性微粉末として塩化ナトリウムを配合した比較例１と比べて、スクロースを配合した実施例１の方が、抽出速度が速く、抽出量も多いことが分かった。 As is clear from the results shown in Tables 1 and 2, the extraction rate was higher in Example 1 in which sucrose was blended than in Comparative Example 1 in which sodium chloride was blended as a water-soluble fine powder. It turns out that there are many.
本発明により得られた高分子化合物多孔体が、連続気泡を有する多孔体であるかを確認するため、以下の実験を行った。 In order to confirm whether the polymer compound porous body obtained by the present invention is a porous body having open cells, the following experiment was conducted.
実施例１に準じて、スクロースを含有する高分子化合物溶液を調製した。先の丸いφ20のアルミニウム製の円柱を、このスクロースを含有する高分子化合物溶液に浸漬し、円柱の表面を被膜した。次いで、乾燥して離型し、袋状のサンプルを調製した。 A polymer compound solution containing sucrose was prepared according to Example 1. The round cylinder made of aluminum having a diameter of φ20 was immersed in the polymer compound solution containing sucrose to coat the surface of the cylinder. Subsequently, it dried and released and the bag-shaped sample was prepared.
500mlビーカーに水道水（20℃）を入れて袋状サンプルを浸漬し、１時間おきに水を交換してスクロースを抽出し、７時間後、乾燥して、袋状の高分子化合物多孔体を得た。 Tap water (20 ° C) into a 500ml beaker, immerse the bag-shaped sample, change the water every other hour to extract sucrose, and after 7 hours, dry the bag-shaped polymer compound porous body. Obtained.
得られた袋状の高分子化合物多孔体の中に水を入れ、24時間放置し、その後表面の水漏れを目視で確認した。その結果、水漏れは確認できなかった。 Water was put into the obtained bag-shaped polymer compound porous body and left standing for 24 hours, and then water leakage on the surface was visually confirmed. As a result, water leakage could not be confirmed.
得られた袋状の高分子化合物多孔体の袋内に空気が残るように、水中に没し、袋の口を閉じて、袋状の高分子化合物多孔体を押した。その結果、袋状の高分子化合物多孔体の表面全体から、内部の空気が泡状に透過してくるのを観察できた。 The bag-shaped polymer compound porous body was immersed in water so that air remained in the bag, the bag mouth was closed, and the bag-shaped polymer compound porous body was pushed. As a result, it was observed that the internal air permeated in the form of bubbles from the entire surface of the bag-like polymer compound porous body.
従って、本発明の連続気泡を有する高分子化合物多孔体は、水を透過しないが、気体を透過することが分かった。 Accordingly, it was found that the polymer compound porous body having open cells of the present invention does not transmit water but transmits gas.
本発明は、耐食性の製造装置を必要とせず、効率的に連続気泡を有する多孔質の高分子化合物を製造することができる。 The present invention does not require a corrosion-resistant production apparatus, and can efficiently produce a porous polymer compound having open cells.
また、本発明方法により得られた連続気泡を有する高分子多孔体は、水を透過しないが、気体を透過する性質を有しているので、例えば、蒸れないゴム手袋、紙おむつ用シート部材、救急絆創膏用シート部材等に応用することが可能である。 Further, the polymer porous body having open cells obtained by the method of the present invention does not transmit water, but has a property of transmitting gas. For example, rubber gloves that do not get steamed, sheet members for disposable diapers, first aid, etc. It can be applied to a sheet member for adhesive bandages.
Claims (4)
2. The production method according to claim 1, wherein the means for removing fine powdered saccharides from the saccharide-containing thermoplastic elastomer is an extraction means using water.
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