JP5183525B2 - Method for producing carbon aggregate molded product - Google Patents
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- JP5183525B2 JP5183525B2 JP2009047568A JP2009047568A JP5183525B2 JP 5183525 B2 JP5183525 B2 JP 5183525B2 JP 2009047568 A JP2009047568 A JP 2009047568A JP 2009047568 A JP2009047568 A JP 2009047568A JP 5183525 B2 JP5183525 B2 JP 5183525B2
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Description
本発明は、カーボン凝結体から成る電磁誘導加熱が可能な炊飯釜などの調理器に関するもので、更に詳しくは熱硬化性樹脂を結合材に用いたカーボン粉粒との混合物が主体の圧縮成形における成形用金型からの成形品の脱型方法（カーボン凝結体成形品の製造方法）と、それによって得られるカーボン凝結体成形品に関する。 The present invention relates to a cooker such as a rice cooker capable of electromagnetic induction heating made of a carbon aggregate, and more specifically, in compression molding mainly composed of a mixture of carbon particles using a thermosetting resin as a binder. The present invention relates to a method for removing a molded product from a molding die (a method for producing a carbon aggregate molded product) and a carbon aggregate molded product obtained thereby.
電磁誘導加熱調理器であるコンロや炊飯器は、高周波磁場発生装置である誘導加熱コイルが発生する渦電流によって磁性体金属である鉄やステンレスなどが発熱する電磁誘導加熱を調理器として利用したものであり、食品の速やかで均一加熱を達成するためにアルミニウムや銅などを積層したクラッド材を鍋状の成形品を調理器として用いていた。しかし、クラッド材は鍋や釜などに絞り加工するものであり、形状の自由度に制限を伴い、さらに平滑な表面を備えることから、フッ素樹脂などの耐熱樹脂塗装面との接着面が剥離し易いという不具合もあった。 Stoves and rice cookers that are electromagnetic induction heating cookers use electromagnetic induction heating that generates heat from magnetic metal such as iron or stainless steel due to eddy currents generated by induction heating coils that are high-frequency magnetic field generators. In order to achieve rapid and uniform heating of the food, a clad material laminated with aluminum, copper, or the like was used as a cooker. However, the clad material is drawn into pots and pots, and is limited in the degree of freedom of shape and has a smoother surface, so the adhesive surface with the heat-resistant resin coating surface such as fluororesin peels off. There was also a problem that it was easy.
このため、従来の鉄やステンレスなどに代わる電磁誘導加熱調理器の素材として、優れた導電性と誘電性と高い熱伝導度を有しているカーボン凝結体の使用が提案されている（例えば、特許文献１参照）。 For this reason, the use of carbon aggregates having excellent conductivity, dielectric properties and high thermal conductivity has been proposed as a material for electromagnetic induction heating cookers that replace conventional iron and stainless steel (for example, Patent Document 1).
また、棒柱状に加圧して凝縮させたカーボン圧縮体の切削加工物が提案されており、カーボン素材が高温での調理器具として有効であることが述べられている（例えば、特許文献２参照）。 Further, a cut product of a carbon compression body that has been pressed and condensed into a columnar shape has been proposed, and it is stated that a carbon material is effective as a cooking utensil at a high temperature (for example, see Patent Document 2). .
上述の調理器具の製造方法によれば、コークスなどのカーボン粉粒にフェノールやピッチなどの高炭素含有物である結合材を主体とする混合物を成形し、これを無酸素雰囲気下の１０００〜３０００℃で加熱してカーボン凝結体を得た後、任意の形状に切削加工するものである。しかし、カーボン焼結体を切削加工して任意の形状に加工することは、切削の大半を占める容器の凹状を成す中空部分にある素材の廃棄が多く、加工工数も大きい、という課題があった。また、カーボン圧縮体に内在する気孔などの欠陥を事前に検知することが困難で、切削によって露出して意匠および強度などの諸特性に悪影響を及ぼすことになる。 According to the above-described method of manufacturing a cooking utensil, a mixture mainly composed of a binder that is a high carbon content such as phenol or pitch is formed on carbon particles such as coke, and this mixture is 1000 to 3000 in an oxygen-free atmosphere. After heating at ℃ to obtain a carbon aggregate, it is cut into an arbitrary shape. However, cutting the carbon sintered body into an arbitrary shape has the problem that the material in the hollow part of the concave portion of the container that occupies most of the cutting is discarded, and the number of processing steps is large. . In addition, it is difficult to detect defects such as pores in the carbon compression body in advance, and it is exposed by cutting and adversely affects various properties such as design and strength.
これらの課題を解決する手段として、カーボン粉粒とフェノール樹脂の原料液やタールピッチなどの結合材との混合物である成形材料を金型内に注入して加圧して賦型した後、得られた成形品を焼成処理することにより、鍋状に成形されたカーボン凝結体を得る手段が提案されている（例えば、特許文献３参照）。 As a means to solve these problems, it is obtained after injecting a molding material, which is a mixture of carbon powder and a binder material such as a phenolic resin raw material liquid and tar pitch, into a mold and pressurizing and molding. There has been proposed a means for obtaining a carbon aggregate formed into a pan shape by firing the molded product (see, for example, Patent Document 3).
この方法によれば、金型に注入したカーボンなどの混合物から成る成形材料の最終充填部が金型の合わせ面として金型内ガスを当該部位から円滑に排出しながら、金型内の狭い空隙を流動して充填させることによって、均質な物性を有する成形品を得る。成形材料が高い流動性を具備することが重要で、前記成形材料の凝集回避と低粘度化を促すために、結合材の混入量を多くするように調整することになる。 According to this method, the final filling portion of the molding material composed of a mixture of carbon or the like injected into the mold serves as a mating surface of the mold and smoothly discharges the gas in the mold from the portion, while narrow gaps in the mold. Is flowed and filled to obtain a molded product having uniform physical properties. It is important that the molding material has high fluidity, and in order to promote aggregation avoidance and lower viscosity of the molding material, adjustment is made to increase the mixing amount of the binder.
しかし、上述のカーボン粉粒と結合材のフェノール樹脂を混合した成形材料は、金型底部に配設して金型と密着してせん断応力を受けながら流動する際に壁面と並行に配向するうえ、熱硬化性樹脂の含有量が多いことから該成形材料の硬化収縮が大きくなり、金型との嵌合力を向上させて脱型が困難になるという課題があった。 However, the molding material in which the above-mentioned carbon particles and a phenolic resin as a binder are mixed is oriented at the same time as the wall surface when flowing while receiving shear stress by being placed in the mold bottom and in close contact with the mold. Further, since the content of the thermosetting resin is large, the curing shrinkage of the molding material is increased, and there is a problem that it is difficult to remove the mold by improving the fitting force with the mold.
上記課題には金型と成形品の離型性を促して密着を回避する手段があり、例えば、金型にナノレベルの離型膜として表面エネルギーを制御した撥水撥油性のフッ化炭素系化学吸着単分子膜を配する方法が提案されている（例えば、特許文献４参照）。 The above-mentioned problems include means for promoting mold releasability between the mold and the molded product to avoid adhesion. For example, a water- and oil-repellent fluorocarbon system in which the surface energy is controlled as a nano-level release film on the mold. A method of arranging a chemisorbed monomolecular film has been proposed (see, for example, Patent Document 4).
また、金型との間に柔軟性に富むエラストマーフィルムから成るインフレーション膜を配して離型させる方法も提案されている（例えば、特許文献５参照）。 In addition, a method has also been proposed in which an inflation film made of a flexible elastomer film is disposed between the mold and released (for example, see Patent Document 5).
さらに、密閉した金型内に粉体離型剤を導入するとともに供給路と対面にある排出路から排気して金型表面に塗布する手段が提案されている（例えば、特許文献６参照）。 Furthermore, means for introducing a powder release agent into a closed mold and exhausting it from a discharge path facing the supply path and applying it to the mold surface has been proposed (see, for example, Patent Document 6).
しかし、これらの上記特許文献４〜６の手段は、成形材料が樹脂層を形成しながら流動する際に離型剤が剥離したり、移行したりするので、成形品表面に離型剤が残留し難く、金型との密着増加に伴ったノックアウトピンなどによる脱型時に受ける局部的な応力負荷による成形品の取り出しに、変形に伴う損傷軽減に対する有効な手段に至らない。 However, in these means of Patent Documents 4 to 6, since the mold release agent peels off or migrates when the molding material flows while forming the resin layer, the mold release agent remains on the surface of the molded product. It is difficult to take out a molded product due to a local stress load received during demolding with a knockout pin or the like accompanying an increase in close contact with the mold, and thus cannot be an effective means for reducing damage due to deformation.
しかも、無酸素雰囲気の高温で焼成処理を施す際の凝結体成形品表面には熱硬化性樹脂の炭化に伴って微細な気孔が生成されるが、該凝結体成形品表面に施す各種塗装が前記気孔に充分な塗料の含浸が行われないことから、アンカー効果による塗膜密着が不十分となり、剥離しやすいという課題を負うことになる。 Moreover, fine pores are generated along with the carbonization of the thermosetting resin when the baking treatment is performed at a high temperature in an oxygen-free atmosphere. Since the pores are not sufficiently impregnated with the coating material, the adhesion of the coating film due to the anchor effect is insufficient, and the problem of easy peeling is incurred.
この発明は、上記のような課題を解決するためになされたもので、成形品の脱型に要する応力の負荷を軽減して円滑に行うことができるカーボン凝結体成形品の製造方法及びカーボン凝結体成形品を提供する。 The present invention has been made in order to solve the above-described problems, and can provide a method for producing a carbon aggregate molded article that can be smoothly performed while reducing the stress load required for demolding the molded article, and carbon agglomeration. Provide body molded products.
この発明に係るカーボン凝結体成形品の製造方法は、カーボン粉粒と熱硬化性高炭素含有化合物が主体の混合物である成形材料を用いる圧縮成形の金型に、易分解性の繊維状物質から成る伸縮性を備えた不織布を配設した状態で、加圧する成形工程を備えて成るものである。 The method for producing a carbon agglomerated molded article according to the present invention is based on a method of forming an easily decomposable fibrous substance into a compression mold using a molding material mainly composed of carbon powder particles and a thermosetting high carbon-containing compound. In the state where the stretchable non-woven fabric is provided, a molding process is performed to pressurize the nonwoven fabric.
この発明に係るカーボン凝結体成形品の製造方法は、カーボン粉粒と熱硬化性高炭素含有化合物が主体の混合物である成形材料を用いる圧縮成形の金型に、易分解性の繊維状物質から成る伸縮性を備えた不織布を配設した状態で、加圧する成形工程を備えるので、成形品の脱型に要する応力の負荷を軽減して円滑に行うことができる。 The method for producing a carbon agglomerated molded article according to the present invention is based on a method of forming an easily decomposable fibrous substance into a compression mold using a molding material mainly composed of carbon powder particles and a thermosetting high carbon-containing compound. Since the forming step of pressurizing is provided in a state in which the nonwoven fabric having stretchability is provided, it is possible to reduce the stress load required for demolding the molded product and smoothly carry out.
実施の形態１．
先ず、本実施の形態の概要を説明する。本実施の形態は、カーボン粉粒と結合材であるフェノール樹脂などの高炭素含有高分子の混合物を、加温した金型に投入して圧縮成形して得た圧縮成形品を無酸素状態で炭化して得るカーボン凝結体成形品から成る炊飯釜の製造に係る圧縮成形における金型との脱型方法に関する。
Embodiment 1 FIG.
First, an outline of the present embodiment will be described. In the present embodiment, a compression molded product obtained by compressing a mixture of carbon particles and a high carbon content polymer such as a phenol resin as a binder into a heated mold is in an oxygen-free state. The present invention relates to a demolding method with a mold in compression molding related to the manufacture of a rice cooker made of a carbon aggregate molded product obtained by carbonization.
カーボン粉粒と結合材である熱硬化性樹脂との混合物を加温した金型に投入して圧縮成形する炊飯釜などの場合、金型の抜き勾配が極めて小さいうえ、成形品が硬化収縮に伴って金型面との嵌合力が強くなって脱型が困難になる。 In the case of a rice cooker, etc., in which a mixture of carbon particles and a thermosetting resin as a binder is put into a heated mold and compression molded, the mold draft is extremely small and the molded product is cured and contracted. Along with this, the fitting force with the mold surface becomes strong and it becomes difficult to remove the mold.
本実施の形態は、金型の表面を伸縮性のある不織布で上型を覆って圧縮成形に供することにより、金型から成形品を容易に脱型するようにしたものである。 In the present embodiment, the molded product is easily removed from the mold by covering the upper mold with a stretchable nonwoven fabric and subjecting the mold to compression molding.
本実施の形態に基づく具体的な成形工程を含むカーボン凝結体成形品の製造方法は、以下の通りである。
（１）成形温度である約１５０℃に加温した圧縮成形用金型を伸縮性のある不織布で覆う；
（２）下型内に原料混合物を投入して上型を閉塞して成形、釜形状に賦型する；
（３）金型を開放、成形品を取り出す；
（４）圧縮成形した釜を無酸素状態雰囲気下で、約１２００℃まで段階的に昇温して有機物を分解、飛散させる。
A method for producing a carbon aggregate molded article including a specific molding step based on the present embodiment is as follows.
(1) Covering a compression molding mold heated to a molding temperature of about 150 ° C. with a stretchable nonwoven fabric;
(2) The raw material mixture is put into the lower mold, the upper mold is closed and molded, and shaped into a pot shape;
(3) Open the mold and take out the molded product;
(4) The temperature of the compression-molded kettle is gradually increased to about 1200 ° C. in an oxygen-free atmosphere to decompose and scatter organic matter.
カーボン粉粒の結合剤であるフェノール樹脂などの高炭素含有熱硬化性樹脂が、金型内で相応の硬化に至ったと判断された段階で行う成形品の脱型は、硬化に要する高温状態を維持してガラス転移温度に至らず、十分な強度が発現しないままで成されることが多い。 Demolding a molded product when a high carbon content thermosetting resin such as phenolic resin, which is a binder for carbon particles, has been determined to have achieved appropriate curing in the mold, should be performed at a high temperature required for curing. In many cases, the glass transition temperature is not maintained and a sufficient strength is not exhibited.
この状態で金型から脱離するための応力を受けた成形品の壁内に亀裂発生を来し、硬化反応の副生成物である水蒸気や未反応の低分子物、さらに結合剤の分解ガスが焼成段階で前記亀裂部分に集中してフクレやクラックの発生を来す。 In this state, cracks occur in the wall of the molded product that has been subjected to stress for detachment from the mold, and steam, unreacted low-molecular substances, which are by-products of the curing reaction, and decomposition gas of the binder However, it concentrates on the cracked part in the firing stage and causes blisters and cracks.
本実施の形態は、結合材の硬化とともに成形品の嵌合力が増加する上金型からの脱型時に発生する応力負荷の軽減を目的に、金型と成形品の密着を抑制するために繊維状の薄膜として不織布を配設するものであり、前記硬化における熱硬化性樹脂の収縮に伴う嵌合力を低減させ、金型との密着部分を抑制して脱型時の滑りを容易とする作用がある。従って、成形品の脱型時に壁面が受ける引張りやせん断応力を低減して、成形品の壁内の亀裂や表面のフクレなどの解消を促す効果を生む。 This embodiment uses a fiber to suppress the adhesion between the mold and the molded product for the purpose of reducing the stress load generated when the mold is removed from the upper mold where the fitting force of the molded product increases as the binder is cured. A non-woven fabric is disposed as a thin film, which reduces the fitting force associated with the shrinkage of the thermosetting resin in the curing, and suppresses the close contact portion with the mold to facilitate slipping during demolding There is. Therefore, the tensile force and shear stress received by the wall surface when the molded product is removed are reduced, and the effect of promoting the elimination of cracks in the wall of the molded product and swelling of the surface is produced.
また、金型に配設した不織布に結合材である熱硬化性樹脂が含浸するので、得られた成形品を無酸素雰囲気で焼成処理によって得たカーボン凝結体成形品には、脆弱な引っ掻きや摩耗を来し易い結合材起源のカーボンを多く含む気孔の少ない密な状態を成す表面層を排除し、気孔を多く含んだ層が形成される。これは、具材との密着防止を目的に施すフッ素樹脂などの塗料含浸を促して、アンカー効果による塗膜密着性を向上させる効果を生む。 In addition, since the thermosetting resin as the binder is impregnated into the nonwoven fabric disposed in the mold, the carbon aggregate molded product obtained by baking the obtained molded product in an oxygen-free atmosphere has fragile scratches and This eliminates the surface layer in a dense state with a small amount of pores containing a large amount of carbon originating from the binder that easily wears, and forms a layer containing a large amount of pores. This promotes the impregnation of a paint such as a fluororesin for the purpose of preventing adhesion to the ingredients, and produces an effect of improving the adhesion of the coating film due to the anchor effect.
圧縮成形に供する金型に、脱型を容易にする易分解性の繊維状物質であるパルプ繊維を抄造して得た伸縮性を備える不織布を配設し、カーボン粉粒と熱硬化性高炭素含有化合物であるフェノール樹脂の混合物によるパンの成形について、以下に詳述する。 A non-woven fabric with elasticity obtained by making pulp fiber, which is an easily decomposable fibrous material that facilitates demolding, is placed in a mold for compression molding, and carbon particles and thermosetting high carbon The molding of bread using a mixture of phenolic resins that are contained compounds will be described in detail below.
まず、成形品の脱型を円滑に行うため、金型形状に近似して伸縮性を備える不織布の製造手段について述べる。１〜３０ｍｍの不均一な長さで直径が約１０μｍの綿状を呈するパルプ繊維を水中で撹拌することによる水のせん断力を受けて解繊し、均一分散したスラリー状の分散液が得られるので、ここにミクロフィブリル化したセルロース繊維をパルプ繊維に対して０．３％を添加して均一に混合する。 First, in order to smoothly remove a molded product, a means for producing a nonwoven fabric having elasticity similar to a mold shape will be described. A pulp fiber having a non-uniform length of 1 to 30 mm and a cotton shape having a diameter of about 10 μm is defibrated by receiving a shearing force of water by stirring in water to obtain a uniformly dispersed slurry dispersion. Therefore, 0.3% of the microfibrillated cellulose fiber is added to the pulp fiber and mixed uniformly.
次に、カチオン性凝集剤を添加してフロックを形成後、アニオン性凝集剤を用いてフロックの凝集性を高めた状態を確保したスラリー液を作成するので、これを８０メッシュの金網を金型内面と相似形状を備えるフィルターの内面に均一散布して濾過して脱水、さらに、８０℃以下の低温で加熱乾燥をすることによって不織布を得る。 Next, a cationic flocculant is added to form a floc, and then an anionic flocculant is used to create a slurry liquid in which a state in which the floc is enhanced is secured. A non-woven fabric is obtained by uniformly spraying on the inner surface of a filter having a shape similar to the inner surface, filtering and dewatering, and further drying by heating at a low temperature of 80 ° C. or lower.
凝集剤とは汚濁水中に分散している汚濁のもととなる微細粒子を集合させて、沈降・浮上を促進するために用いられる薬剤のことをいう。凝集剤の働きによってできる微細粒子の集合体をフロックと呼ぶ。 The aggregating agent refers to a drug used for collecting fine particles that are the source of pollution dispersed in the polluted water to promote sedimentation and levitation. An aggregate of fine particles formed by the action of the flocculant is called floc.
得られる不織布は、坪量が３０〜５０ｇ／ｍ２になるよう、金網への散布量を調整することによって、圧縮成形後の不織布厚さを限定する。また、パルプ繊維はミクロフィブリル化セルロースによって相互が結合して成るので、繊維の配向を柔軟に変化して前記不織布を圧縮成形に供する金型嵌合時の伸縮性を維持して密着を容易とすることができた。 The nonwoven fabric obtained limits the nonwoven fabric thickness after compression molding by adjusting the amount of application to the wire mesh so that the basis weight is 30 to 50 g / m 2 . In addition, since the pulp fibers are bonded to each other by the microfibrillated cellulose, the orientation of the fibers is changed flexibly, and the nonwoven fabric is subjected to compression molding. We were able to.
次に、圧縮成形によるパン状成形品を得る手段に関し、原料であるカーボン粉粒と液状の結合材との混合物を充填する金型から得られる電磁誘導加熱調理器の製造方法について、以下に詳述する。 Next, regarding a means for obtaining a bread-shaped product by compression molding, a method for producing an electromagnetic induction heating cooker obtained from a mold filled with a mixture of raw material carbon particles and a liquid binder will be described in detail below. Describe.
まず、石油コークスを約３０００℃の無酸素状態で焼成してグラファイト化した塊状物を粉砕して得た平均粒径が０．３〜１．０ｍｍのカーボン粉粒物７０部と、ノボラック型のフェノール樹脂３０部と、を混練して成形材料とした。 First, 70 parts of carbon particles having an average particle size of 0.3 to 1.0 mm obtained by pulverizing a mass of petroleum coke fired in an oxygen-free state at about 3000 ° C. and graphitized, and a novolac type 30 parts of phenol resin was kneaded to obtain a molding material.
上記成形材料は、約１６０℃に加温した下金型の底面に均一散布した後、成形品が硬化時の収縮などで密着し易い上型表面に不織布を保持した状態で閉塞、加圧することによって賦型する。 The above molding material is uniformly sprayed on the bottom surface of the lower mold heated to about 160 ° C., and then the molded product is closed and pressed in a state where the nonwoven fabric is held on the upper mold surface which is easily adhered due to shrinkage at the time of curing. Mold by.
投入した成形材料は底面部で溶融後、側壁部を上昇して金型内を充填する。この時、上下金型が当接するパーティング面から金型内に残存する空気と成形材料に残存する低分子物やフェノール樹脂の硬化に伴う副生成物などのガスを排出するが、金型の一部から排気ポンプによって減圧状態を得ると、円滑な充填状態が得られるので、なお良い。 The injected molding material is melted at the bottom surface, and then the side wall is raised to fill the mold. At this time, gas such as air remaining in the mold and low-molecular substances remaining in the molding material and by-products accompanying the curing of the phenol resin are discharged from the parting surface where the upper and lower molds abut. It is even better if a reduced pressure state is obtained from a part by an exhaust pump because a smooth filling state is obtained.
金型はフェノール樹脂の硬化が完了する５〜６分後に開放し、成形品を取り出す。得られた成形品の表面には不織布にフェノール樹脂が含浸した状態で密着している。しかし、金型開放に最も抵抗となる側壁では金型との当接面にまで至らず、また、底面部には金型との当接面まで含浸したフェノール樹脂が及んでいるものの、殆ど、密着すること無しに成形品を脱離することが出来た。 The mold is opened 5 to 6 minutes after the phenol resin is completely cured, and the molded product is taken out. The surface of the obtained molded product is in close contact with the nonwoven fabric impregnated with a phenol resin. However, the side wall that is most resistant to mold opening does not reach the contact surface with the mold, and the bottom surface portion is almost covered with phenol resin impregnated to the contact surface with the mold, The molded product could be removed without sticking.
次に、前記成形品を焼成して有機物の分解および炭素化を行うことによって、電磁誘導加熱が可能な素材を備えたパンとなるように焼成処理を行った。 Next, the molded product was baked to decompose and carbonize the organic matter, thereby performing a baking process so as to obtain a bread having a material capable of electromagnetic induction heating.
上述の成形品は、窒素雰囲気の電気炉内で加熱するが、成形時に残存した内部応力の解放による膨張挙動と焼成時の分解生成物放散に伴う収縮挙動によるクラックが発生しないように、段階的に温度の上昇を制御することが肝要であった。 The above-mentioned molded product is heated in an electric furnace in a nitrogen atmosphere, but stepwise so that cracks due to expansion behavior due to release of internal stress remaining at the time of molding and shrinkage behavior due to dissipation of decomposition products during firing do not occur. It was important to control the temperature rise.
このため、焼成処理は、３００℃までを３〜５℃／ｈｒ、６００℃までを１〜３℃／ｈｒ、９５０℃までを５〜１０℃／ｈｒ の昇温速度で焼成した。得られたカーボン凝結体には、表面に密着していた不織布が分解して飛散した痕跡としての微細な凹凸があるため、これをブラスト処理などにより排除して、平滑面を確保した。 For this reason, the baking treatment was performed at a heating rate of 3 to 5 ° C / hr up to 300 ° C, 1 to 3 ° C / hr up to 600 ° C, and 5 to 10 ° C / hr up to 950 ° C. The obtained carbon agglomerates had fine irregularities as traces of the non-woven fabric that was in close contact with the surface being decomposed and scattered, and this was eliminated by blasting or the like to ensure a smooth surface.
以上のカーボン凝結体から成る成形品の表面にはフェノール樹脂の分解物が気散して生成する気孔が存在し、さらに耐摩耗性に劣るうえ、調理の際に調理物が密着して調理に不具合を生じるため、カーボン凝結体の表面を保護する塗装を施す必要がある。内面には調理物を付着し難い態様を確保するためにフッ素樹脂の塗装を、外面には耐摩耗性と耐熱性に優れるシリコン樹脂を塗布し、調理器具として用いることになる。 On the surface of the molded product composed of the above carbon aggregates, there are pores generated by the decomposition of phenol resin decomposition products, and it is inferior in wear resistance. In order to cause defects, it is necessary to apply a coating that protects the surface of the carbon aggregate. The inner surface is coated with a fluororesin in order to ensure that the food is difficult to adhere, and the outer surface is coated with a silicone resin having excellent wear resistance and heat resistance to be used as a cooking utensil.
従って、該成形品の壁面内にクラックなどが生じていると、その部分が膨れて平滑な調理面を確保できない、という不具合が生じることになる。本実施の形態による大きな粒径のカーボン粉粒を用いた成形品の場合、成形直後の内層部では、大きな粒子が凝集し易い中央部分の強度が脆弱である上、金型温度が伝播しにくいために反応が遅延するうえ、脱型後の製品の温度も高いことから亀裂を発生しやすい。 Therefore, if a crack or the like is generated in the wall surface of the molded product, there is a problem that the portion swells and a smooth cooking surface cannot be secured. In the case of a molded product using carbon particles having a large particle diameter according to the present embodiment, the inner layer portion immediately after molding has a weak central portion where large particles tend to aggregate, and the mold temperature is difficult to propagate. As a result, the reaction is delayed and the temperature of the product after demolding is high, so cracks are likely to occur.
不織布を金型に保持せずに成形した成形品の凝結体では、２５０℃の雰囲気に投入して急速な昇温によって調理面に５〜２０ｍｍ程度のフクレを発生したが、本実施の形態による成形品には変形を来すことがなく、また、裁断して壁面内の目視観察によっても亀裂を確認できなかった。 In the agglomerate of the molded product formed without holding the nonwoven fabric in the mold, it was put into an atmosphere at 250 ° C. and a rapid rise in temperature caused a swelling of about 5 to 20 mm on the cooking surface. The molded product was not deformed, and it was not possible to confirm cracks by cutting and visually observing the wall surface.
実施の形態１をまとめると、以下のようになる。
この実施の形態に係るカーボン凝結体の製造方法は、カーボン粉粒と熱硬化性高炭素含有化合物が主体の混合物である成形材料を用いる圧縮成形の金型に、易分解性の繊維状物質から成る伸縮性を備えた不織布を配設した状態で、加圧する成形工程を備えて成ることを特徴とする。
The first embodiment is summarized as follows.
The method for producing a carbon aggregate according to this embodiment is obtained from an easily decomposable fibrous substance into a compression mold using a molding material mainly composed of carbon powder and a thermosetting high carbon-containing compound. It is characterized by comprising a molding step of applying pressure in a state in which a non-woven fabric having elasticity is provided.
また、易分解性の繊維状物質が、草木繊維であるパルプおよびエステル系樹脂から成ることを特徴とする。 Further, the easily decomposable fibrous substance is composed of pulp and ester resin which are plant fibers.
また、伸縮性を備えた不織布が、成形品の内面に近似した形状を成すように抄造されて成ることを特徴とする。 In addition, the nonwoven fabric having elasticity is formed by making paper so as to have a shape approximate to the inner surface of the molded product.
また、伸縮性を備える不織布の抄造が、ミクロフィブリル化したセルロースを結合材として用いて成ることを特徴とする。 In addition, the production of a nonwoven fabric having stretchability is characterized by comprising microfibrillated cellulose as a binder.
また、伸縮性を備えた不織布が、金型に載置した状態で熱硬化性樹脂を含浸させて用いることを特徴とする。 Further, the nonwoven fabric having elasticity is used by being impregnated with a thermosetting resin in a state of being placed on a mold.
実施の形態２．
繊維状に加工したフェノール樹脂または籾殻繊維を燻蒸した繊維によって脱型を容易にする不織布を作成し、これを圧縮成形に供する金型に配設して、カーボン粉粒とフェノール樹脂の混合物によるパン状成形品の成形と調理器具となる凝結体の製造方法について、以下に詳述する。
Embodiment 2. FIG.
A non-woven fabric that facilitates demolding is created by using a phenol resin processed into a fiber or a fiber fumigated from rice husk fibers, and this is placed in a mold for compression molding, and a bread made of a mixture of carbon powder and phenol resin. A method for producing a molded product and a method for producing a condensate serving as a cooking utensil will be described in detail below.
まず、成形品の脱型を円滑に行うため、金型形状に近似して伸縮性を備える不織布の製造方法について述べる。籾殻を２枚の円板に挟んですり潰すようにして繊維を含む粉末を取り出し、これを水洗しながら粉末を除去して繊維分のみを回収する。前記繊維分は４５０℃〜８００℃、好ましくは６００℃の窒素置換した無酸素雰囲気下で加熱する燻蒸処理を行うことによって、ＳｉＯまたはＳｉＯ２を４５〜５５％含有する籾殻炭化物繊維が得られる。 First, a method for producing a nonwoven fabric having elasticity that approximates the shape of a mold in order to smoothly remove a molded product will be described. The powder containing fibers is taken out by crushing rice husks between two discs, and the powder is removed while washing with water to collect only the fiber. By performing a fumigation treatment in which the fiber content is heated in an oxygen-free atmosphere with nitrogen substitution at 450 ° C. to 800 ° C., preferably 600 ° C., rice husk carbide fibers containing 45 to 55% of SiO or SiO 2 are obtained.
上記籾殻炭化物繊維は水中で撹拌してスラリー状の分散液を得た後、ミクロフィブリル化したセルロース繊維を前記籾殻炭化物繊維に対して０．３％を添加して均一に混合、カチオン性凝集剤を用いてフロックを形成した後、アニオン性凝集剤を用いてフロックの凝集性を高めた状態を確保した第１のスラリー液を作成する。 The rice husk carbide fiber is stirred in water to obtain a slurry-like dispersion, and then the microfibrillated cellulose fiber is added to 0.3% of the rice husk carbide fiber and mixed uniformly to form a cationic flocculant. After the floc is formed using, a first slurry liquid in which a state in which the floc cohesiveness is enhanced is secured using an anionic flocculant is prepared.
一方、上記第１のスラリー液とは別に、同様手段でポリエステル繊維の分散液にミクロフィブリル化セルロース繊維を前記ポリエステル繊維の０．３％を添加して均一に混合、これにカチオン性凝集剤を添加してフロックを形成後、アニオン性凝集剤を用いてフロックの凝集性を高めた状態を確保した第２のスラリー液を作成する。 On the other hand, apart from the first slurry liquid, a microfibrillated cellulose fiber is added to the polyester fiber dispersion by the same means and 0.3% of the polyester fiber is uniformly mixed, and a cationic flocculant is added thereto. After the formation of flocs by addition, a second slurry liquid in which a state in which the flocs coagulability is enhanced is secured using an anionic flocculant is prepared.
次に、予め作製した８０メッシュの金網を上金型内面と相似形状を備えたフィルターの凹状内面に、第２のスラリー液を均一に散布して濾過、減圧吸引して脱水後、同面上に積層するようにして第２のスラリー液を均一散布して濾過、それを十分に脱水後、８０℃以下の低温で加熱乾燥をすることによって不織布を得た。 Next, a 80-mesh wire mesh prepared in advance is applied to the concave inner surface of a filter having a shape similar to the inner surface of the upper mold, and the second slurry is uniformly dispersed, filtered, suctioned under reduced pressure, and dehydrated. The nonwoven fabric was obtained by uniformly spraying the second slurry liquid so as to be laminated and filtering, sufficiently dehydrating it, and drying by heating at a low temperature of 80 ° C. or lower.
不織布は、第２のスラリー液の坪量が１０〜３０ｇ／ｍ２、第１のスラリー液の坪量が２０〜５０ｇ／ｍ２を成すように金網への散布量を調整し、圧縮成形後の不織布厚さを限定することが肝要である。 After the compression molding, the non-woven fabric is adjusted in the amount applied to the wire mesh so that the basis weight of the second slurry liquid is 10 to 30 g / m 2 and the basis weight of the first slurry liquid is 20 to 50 g / m 2. It is important to limit the thickness of the nonwoven fabric.
ここで用いたポリエステル繊維はミクロフィブリル化セルロースによって相互が強固に結合して成るので、繊維の配向を柔軟に変化して前記不織布を圧縮成形に供する金型嵌合時の伸縮性を維持して密着を容易とすることができる。 Since the polyester fibers used here are firmly bonded to each other by the microfibrillated cellulose, the orientation of the fibers is flexibly changed to maintain the stretchability when fitting the mold for compression molding of the nonwoven fabric. Adhesion can be facilitated.
また、籾殻炭化物繊維の長さが０．１〜２ｍｍである短繊維であっても、含有するＳｉＯまたはＳｉＯ２によってミクロフィブリル化セルロースが吸着しやすい状態を保持して強固なフロックを形成して成るので、下層を成すポリエステル繊維の不織布が減圧吸引によって密と成した繊維間空隙を通過せず、積層して保持された。 Moreover, even if it is a short fiber whose length of rice husk carbide fiber is 0.1 to 2 mm, it maintains a state in which microfibrillated cellulose is easily adsorbed by the contained SiO or SiO 2 to form a strong flock. As a result, the polyester fiber non-woven fabric forming the lower layer did not pass through the dense inter-fiber gap formed by vacuum suction, and was laminated and held.
次に、圧縮成形によってパン状の成形品を得る。まず、石油コークスを約３０００℃でグラファイト化した塊状物の粉砕として得た平均粒径が０．３〜１．０ｍｍのカーボン粉粒物７０部と、ノボラック型のフェノール樹脂３０部と、を混練して成形材料とした。 Next, a bread-shaped molded product is obtained by compression molding. First, 70 parts of carbon particles having an average particle size of 0.3 to 1.0 mm obtained by pulverizing a lump obtained by graphitizing petroleum coke at about 3000 ° C. and 30 parts of a novolac type phenol resin are kneaded. Thus, a molding material was obtained.
成形品が硬化収縮などで密着し易い上金型面に籾殻炭化物繊維を保持するポリエステル繊維の抄造面を当接するように保持した後、成形材料を加温した下金型の底面に均一散布して閉塞、加圧することによって賦型する。 After holding the paper making surface of polyester fiber holding rice husk carbide fiber on the upper mold surface where the molded product is easy to adhere due to cure shrinkage, etc., uniformly spray the molding material on the bottom surface of the heated lower mold And then mold by pressurizing and pressurizing.
投入した成形材料は底面部で溶融後、側壁部を上昇して金型内を充填するが、この時、上下金型の当接面に設けた溝から、金型内の残存空気と成形材料に残存する低分子物やフェノール樹脂の硬化に伴う副生成物などのガスを、真空ポンプなどによって減圧状態を得ながら排気すると、円滑な充填状態が得られるので、好ましい。 The injected molding material is melted at the bottom, and then the side wall is raised to fill the mold. At this time, the remaining air in the mold and the molding material are filled from the grooves provided on the contact surfaces of the upper and lower molds. It is preferable to exhaust the gas such as low-molecular substances remaining in the resin and by-products accompanying the curing of the phenol resin while obtaining a reduced pressure state with a vacuum pump or the like because a smooth filling state can be obtained.
金型は約１６０℃に加温されており、フェノール樹脂の硬化が完了する５〜６分後に開放し、成形品を取り出す。成形品は不織布にフェノール樹脂が含浸して密着しているが、金型当接面まで透過せず、金型開放の成形材料の嵌合による抵抗を緩和する効果を生み出し、密着すること無しに成形品を脱離することが出来た。 The mold is heated to about 160 ° C., opened 5 to 6 minutes after the phenol resin is completely cured, and the molded product is taken out. The molded product is impregnated with a non-woven fabric with phenolic resin, but does not penetrate to the mold contact surface. The molded product could be detached.
次に、前記成形品は電磁誘導加熱を可能とするよう、焼成処理を行った。成形品は窒素雰囲気で加熱し、内部応力の解放による膨張と分解物放散による収縮を抑制してクラック発生を防止するため、３００℃までを３〜５℃／ｈｒ、６００℃までを１〜３℃／ｈｒ、１３５０℃までを５〜１０℃／ｈｒの段階的な昇温速度とした。 Next, the molded product was baked to enable electromagnetic induction heating. The molded product is heated in a nitrogen atmosphere to suppress cracking by suppressing expansion due to release of internal stress and shrinkage caused by decomposition product decomposition. C./hr up to 1350.degree. C. was a stepwise temperature increase rate of 5-10.degree. C./hr.
得られたカーボン凝結体は、脱型時の壁面内層における亀裂発生を確認する２５０℃まで急速に加温を施しても、フクレの発生を来すことがなく、また、裁断して壁面内の目視観察によっても亀裂を確認できなかった。 The obtained carbon agglomerate does not cause blistering even if it is rapidly heated to 250 ° C., which confirms the occurrence of cracks in the inner wall layer during demolding. No cracks could be confirmed by visual observation.
以上のカーボン凝結体から成る成形品には表面に密着していた不織布が分解して飛散した痕跡である微細な凹凸と耐摩耗性に劣るポリエステル繊維の炭化物があり、これをブラスト処理などで排除し、籾殻炭化物繊維が露出した平滑面を確保した。 Molded products composed of the above carbon aggregates contain fine irregularities that are traces of the non-woven fabric that was in close contact with the surface being decomposed and scattered, and polyester fiber carbides that are inferior in wear resistance. And a smooth surface with exposed rice husk carbide fibers was secured.
該凝結体には分解物の飛散痕である気孔が存在するため、調理に不具合を生じないように、内面には調理物を付着し難い態様を確保するフッ素樹脂の塗装を、外面には耐摩耗性と耐熱性に優れるシリコン樹脂を塗布し、調理器具として用いることになる。 Since the aggregates have pores that are scattered traces of decomposed products, the inner surface is coated with a fluororesin to ensure that the food is difficult to adhere, and the outer surface is resistant to cooking. A silicon resin excellent in wear and heat resistance is applied and used as a cooking utensil.
該成形品は、上金型と嵌合した不織布の金型との反当接面にあって成形品の内面を形成する籾殻炭化物繊維を備えた面は、無酸素状態の高温での焼成処理において、フェノール樹脂などの分解生成物などと反応して強固なＳｉＣを生成して調理面の基材として優れた剛性を備えて、調理時にヘラなどの調理道具による摩擦や圧接などの負荷による損傷への耐性に優れるように改質されるので、好ましい。 The molded article is on the surface that is opposite to the non-woven mold fitted with the upper mold, and the surface provided with the chaff carbide fiber forming the inner surface of the molded article is subjected to an oxygen-free high-temperature firing treatment. , Which produces strong SiC by reacting with decomposition products such as phenolic resin and has excellent rigidity as a base material for cooking surfaces, and damage caused by loads such as friction and pressure welding with a cooking tool such as a spatula during cooking This is preferable because it is modified so as to have excellent resistance to aging.
同様に、基材の強度が向上したことによって、調理具として供するために行う上述の表面塗装において、塗膜の密着性が向上する効果を得た。籾殻炭化物繊維を具備した不織布は、成形材料が含んでカーボン粉粒間の空隙を充填して余る過剰量のフェノール樹脂を含浸して成るが、前記不織布の厚さは、これを透過するに至らない。従って、籾殻炭化物繊維同士が成した多くの空隙を該凝結体は備えて成り、優れた塗料の含浸性を呈する。 Similarly, by improving the strength of the base material, an effect of improving the adhesion of the coating film was obtained in the above-described surface coating performed for serving as a cooking utensil. A non-woven fabric provided with rice husk carbide fiber is formed by impregnating an excess amount of phenolic resin, which is included in the molding material and filling the voids between the carbon particles, but the thickness of the non-woven fabric penetrates this. Absent. Therefore, the aggregate is provided with many voids formed by rice husk carbide fibers, and exhibits excellent paint impregnation properties.
つまり、塗膜密着性は、耐摩耗性と耐熱性に優れるシリコン樹脂をスプレー塗装の際、塗料がカーボン凝結体の備える気孔内に含浸してアンカー効果により固着して発現する。従って、籾殻炭化物繊維を具備しない不織布を配設した場合、基材への含浸に乏しいうえに脆弱であることから、破壊を伴う塗膜剥離が観察されたのに対し、本実施の形態のカーボン凝結体では、優れた塗料含浸性を呈するうえに基材が強靱であることから高い塗膜密着性を呈する。 That is, the coating film adhesion is manifested when the coating is impregnated into the pores of the carbon aggregates and fixed by the anchor effect when spraying silicon resin having excellent wear resistance and heat resistance. Therefore, when a non-woven fabric without rice husk carbide fibers was disposed, the coating film peeling accompanied by breakage was observed because the base material was poorly impregnated and fragile. The agglomerated material exhibits excellent paint impregnation properties and high coating film adhesion because the substrate is tough.
塗膜の剥離強さの測定は、塗膜のみに１ｍｍ間隔で縦横に１１本の切れ目を碁盤目状に入れ、該面上にテープを密着させて２０回の引き剥しを繰返した後、升目部分の欠損箇所を確認、無欠損の升目の数（ａ／１００）で評価する。その結果を図１に示す。 The peel strength of the coating film was measured by placing 11 cuts vertically and horizontally at a 1 mm interval in a checkerboard pattern on the coating film only, and attaching the tape onto the surface and repeating the peeling 20 times. The missing part of the part is confirmed and evaluated by the number of squares without defect (a / 100). The result is shown in FIG.
図１に示すように、籾殻炭化物繊維を具備しない不織布を配設したものは７８／１００であったが、本実施の形態のカーボン凝結体の場合は全く剥離しない１００／１００の結果であり、優位に優れていることが確認できた。 As shown in FIG. 1, the non-woven fabric without rice husk carbide fiber was 78/100, but the carbon aggregate of the present embodiment is a 100/100 result that does not peel at all. It was confirmed that it was superior.
なお、本実施の形態では、易分解性繊維としてポリエステルを用いたが、これに代えて各種パルプを用いても同様の効果が得られる。また、種子草木の外披から成る繊維を主体としたフロックスから成るスラリー液に代えて、カーボン粉粒と、それと易分解性繊維を結合する接着剤の混合物を用いても、同様の効果が得られる。 In the present embodiment, polyester is used as the easily decomposable fiber, but the same effect can be obtained by using various pulps instead. The same effect can be obtained by using a mixture of carbon powder and an adhesive that binds easily degradable fibers in place of the slurry liquid consisting of Phlox mainly composed of seed vegetation. It is done.
実施の形態２をまとめると、以下のようになる。
この実施の形態に係るカーボン凝結体の製造方法は、カーボン粉粒と熱硬化性高炭素含有化合物の結合材が主体の混合物である成形材料を用いる圧縮成形の金型に、易分解性樹脂繊維と種子草木の外披から成る繊維を含んだ伸縮性を備える不織布を配設した状態で、加圧する成形工程を備えて成ることを特徴とする。
The summary of the second embodiment is as follows.
The method for producing a carbon aggregate according to this embodiment includes an easily decomposable resin fiber in a compression molding mold using a molding material mainly composed of a binder of carbon powder particles and a thermosetting high carbon-containing compound. And a forming step of pressing in a state in which a non-woven fabric having stretchability including fibers composed of seed and vegetation is provided.
また、種子草木の外披から成る繊維が、籾殻繊維を燻蒸したものであることを特徴とする。 In addition, the fiber composed of the seed vegetation is fumigated rice husk fiber.
また、不織布が、成形品の内面形状に近似して抄造されて成ることを特徴とする。 Further, the nonwoven fabric is made by making a paper similar to the inner shape of the molded product.
また、不織布が、易分解性樹脂繊維と種子草木の外披から成る繊維の固定にミクロフィブリル化したセルロースを用いて抄造したものであることを特徴とする。 In addition, the nonwoven fabric is made by using microfibrillated cellulose for fixing fibers composed of easily decomposable resin fibers and seed vegetation.
また、不織布が、易分解性樹脂繊維を抄造したうえに種子草木の外披から成る繊維を積層した混抄紙であることを特徴とする。 In addition, the nonwoven fabric is a mixed paper obtained by making easily degradable resin fibers and laminating fibers made of seed vegetation.
また、不織布が、易分解性樹脂の長繊維を抄造したのちに面方向に負荷をかけて繊維間を密な状態にした後、種子草木の外披から成る短繊維を積層することを特徴とする。 In addition, the non-woven fabric is characterized by laminating short fibers composed of seed vegetation after making a long fiber of an easily decomposable resin and applying a load in the surface direction to close the fiber between the fibers. To do.
この実施の形態に係るカーボン凝結体成形品は、内部がカーボン粉粒と熱硬化性高炭素含有樹脂炭化物の混合体で、表面に籾殻繊維燻蒸物と高炭素含有樹脂炭化物の混合体を配し、最表面に籾殻繊維燻蒸物が高炭素含有樹脂炭化物と複合化しない状態で露出して成ることを特徴とする。 The carbon aggregate molded product according to this embodiment has a mixture of carbon particles and thermosetting high carbon content resin carbide inside, and a mixture of rice husk fiber fumigation and high carbon content resin carbide on the surface. The rice husk fiber fumigation material is exposed on the outermost surface in a state where it is not combined with the high carbon content resin carbide.
また、カーボン粉粒が、コークスを無酸素雰囲気の２６００℃以上の高温で処理して得た黒鉛であることを特徴とする。 The carbon powder is graphite obtained by treating coke at a high temperature of 2600 ° C. or higher in an oxygen-free atmosphere.
Claims (5)
前記金網を用いて抄造した不織布を前記金型の内面に配設する工程と、
カーボン粉粒と熱硬化性炭素含有化合物とが主体の混合物である成形材料を、前記不織布を内面に配設した金型内に投入し、加圧して成形する工程とを備えることを特徴とするカーボン凝結体成形品の製造方法。 Using a wire mesh having a shape close to the inner surface of a compression mold, and making a nonwoven fabric having elasticity with pulp and ester resin as raw materials;
Disposing a non-woven fabric made using the wire mesh on the inner surface of the mold; and
The molding material and carbon powder particles and a thermosetting-carbon-containing compound is a mixture of mainly the nonwoven fabric was poured into a mold which is disposed on the inner surface, that obtain Bei and a step of molding under pressure A method for producing a carbon aggregate molded product, which is characterized.
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