JP2007070769A - Method for producing inorganic fiber-formed material - Google Patents
Method for producing inorganic fiber-formed material Download PDFInfo
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- JP2007070769A JP2007070769A JP2005260829A JP2005260829A JP2007070769A JP 2007070769 A JP2007070769 A JP 2007070769A JP 2005260829 A JP2005260829 A JP 2005260829A JP 2005260829 A JP2005260829 A JP 2005260829A JP 2007070769 A JP2007070769 A JP 2007070769A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 title abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000012784 inorganic fiber Substances 0.000 claims abstract description 35
- 239000011230 binding agent Substances 0.000 claims abstract description 34
- -1 polyoxyethylene Polymers 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000835 fiber Substances 0.000 claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 229920003067 (meth)acrylic acid ester copolymer Polymers 0.000 claims abstract description 10
- 150000005215 alkyl ethers Chemical class 0.000 claims abstract description 10
- 229920001577 copolymer Polymers 0.000 claims abstract description 8
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000000034 method Methods 0.000 abstract description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000010304 firing Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000009987 spinning Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical class CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003985 ceramic capacitor Substances 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 229920003145 methacrylic acid copolymer Polymers 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
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Abstract
Description
本発明は、無機繊維成形体の製造方法に関する。 The present invention relates to a method for producing an inorganic fiber molded body.
従来、例えば携帯電話等に使用される積層セラミックコンデンサーは、水素、一酸化炭素、ナトリウム等の還元物質やアルカリ物質を含む雰囲気下、１４００℃程度で焼成する工程を経て製造されている。このような過酷な焼成から炉を保護するため、アルミナ質繊維成形体からなる炉材が用いられているが、還元物質やアルカリ物質による浸食と加熱、冷却によるスポーリングが激しく、頻繁に補修が必要であった。これらを解決するには、アルミナ含有率が高く、均質で、嵩密度のできるだけ小さい炉材を用いればよいが、通常のアルミナ含有率が７０質量％以上のアルミナ質繊維成形体、すなわちアルミナ質繊維と有機バインダーと無機バインダーを含む水スラリーを抄造した後乾燥して製造されたアルミナ質繊維成形体では、その嵩密度が０．２５程度である（特許文献１）ので、上記雰囲気下における耐久性が十分とはいえなかった。嵩密度をより小さくするには、水スラリーの調製時間を短くする等の方法が考えられるが、均質な繊維成形体が得られにくくなる問題があった。
本発明の目的は、嵩密度が小さく、均質な無機繊維成形体とすることが容易な無機繊維成形体の製造方法を提供することである。 The objective of this invention is providing the manufacturing method of an inorganic fiber molded object with a small bulk density and being easy to make a homogeneous inorganic fiber molded object.
本発明は、無機繊維と有機バインダーと無機バインダーを含む水スラリーを抄造後乾燥する方法において、有機バインダーとして（メタ）アクリル酸エステル共重合体とポリオキシエチレンアルキルエーテルを併用することを特徴とする無機繊維成形体の製造方法である。この場合において、水スラリーの無機繊維の含有率が０．２〜３．０質量％、有機バインダーが０．０１〜０．３質量％、無機バインダーが０．０１〜０．３質量％であること、無機繊維がアルミナ／シリカの質量比が９７／３〜９０／１０のアルミナ質繊維であること、（メタ）アクリル酸エステル共重合体がアクリル酸ブチル共重合体であり、ポリオキシエチレンアルキルエーテルがポリオキシエチレンラウリルエーテルであることが好ましい。 The present invention is characterized in that a (meth) acrylic acid ester copolymer and a polyoxyethylene alkyl ether are used in combination as an organic binder in a method of making and drying a water slurry containing inorganic fibers, an organic binder, and an inorganic binder. It is a manufacturing method of an inorganic fiber molded object. In this case, the inorganic fiber content of the water slurry is 0.2 to 3.0 mass%, the organic binder is 0.01 to 0.3 mass%, and the inorganic binder is 0.01 to 0.3 mass%. That the inorganic fiber is an alumina fiber having an alumina / silica mass ratio of 97/3 to 90/10, the (meth) acrylate copolymer is a butyl acrylate copolymer, and polyoxyethylene alkyl The ether is preferably polyoxyethylene lauryl ether.
本発明によれば、積層セラミックコンデンサー等の焼成炉のように、還元物質又はアルカリ物質を含む高温の雰囲気中に曝されても、また、加熱、冷却を繰り返しても損耗を少なくすることのできる、嵩密度が小さく、均質な無機繊維成形体を容易に製造することができる。 According to the present invention, it is possible to reduce wear even when exposed to a high temperature atmosphere containing a reducing substance or an alkaline substance, or by repeated heating and cooling, as in a firing furnace such as a multilayer ceramic capacitor. In addition, a uniform inorganic fiber molded body having a small bulk density can be easily produced.
無機繊維と有機バインダーと無機バインダーを含む水スラリーを抄造法によりフェルト、ボード等の無機繊維成形体とすることは知られている（特開２００２−３２１９８６号公報）。詳述すれば、底面に網板を備えた箱型容器に水スラリーを流し込み、網の下方で吸引しながら脱水し、網面上のケーキを乾燥する方式、水スラリー中に吸引機構を備えた平網を沈め、吸引して漉き上げたケーキを乾燥する方式、丸網抄造機、長網抄造機等の連続抄造設備を用いる方式等である。ケーキの乾燥は熱風乾燥で行われる。 It is known that an aqueous slurry containing inorganic fibers, an organic binder, and an inorganic binder is formed into an inorganic fiber molded body such as felt or board by a papermaking method (Japanese Patent Laid-Open No. 2002-321986). In detail, the water slurry was poured into a box-type container having a net plate on the bottom, dehydrated while sucking under the net, and the cake on the net surface was dried, equipped with a suction mechanism in the water slurry For example, a method of drying a cake that has been sunk and sucked up by a flat screen, a method using a continuous paper making machine such as a round net paper making machine or a long net paper making machine. The cake is dried by hot air drying.
無機繊維としては、例えばチタニア、アルミナ、シリカ等の酸化物繊維の少なくとも一種が用いられ、中でもアルミナ／シリカの質量比が９７／３〜９０／１０であるアルミナ質繊維が還元物質又はアルカリ物質への耐久性が大きいので好ましい。アルミナ質繊維は、例えばアルミニウム塩水溶液と、シリカゾル分散体と、例えばポリビニルアルコール、カルボキシメチルセルロース、澱粉等の紡糸助剤とを含有し、粘度が３００〜５０００ｍＰａ・ｓである紡糸原液を、０．１〜１．０ｍｍのノズルより液糸として押し出し、１５０〜７００℃の乾燥気流によって乾燥固化させることによって製造することができる（特開２００２−３２１９８６号公報）。 As the inorganic fiber, for example, at least one kind of oxide fiber such as titania, alumina, silica and the like is used, and among these, an alumina fiber having an alumina / silica mass ratio of 97/3 to 90/10 is reduced to a reducing substance or an alkaline substance. Is preferable because of its high durability. The alumina fiber contains, for example, an aluminum salt aqueous solution, a silica sol dispersion, and a spinning aid such as polyvinyl alcohol, carboxymethyl cellulose, and starch, and a spinning stock solution having a viscosity of 300 to 5000 mPa · s. It can be manufactured by extruding as a liquid thread from a nozzle of ˜1.0 mm and drying and solidifying with a dry air flow of 150 to 700 ° C. (Japanese Patent Laid-Open No. 2002-321986).
有機バインダーとしては、（メタ）アクリル酸エステル共重合体とポリオキシエチレンアルキルエーテルを併用する。有機系バインダーの使用量は、無機繊維１００質量部に対して５〜２０質量部が好ましく、１０〜１５質量部がより好ましい。 As the organic binder, a (meth) acrylic acid ester copolymer and polyoxyethylene alkyl ether are used in combination. 5-20 mass parts is preferable with respect to 100 mass parts of inorganic fibers, and, as for the usage-amount of an organic type binder, 10-15 mass parts is more preferable.
（メタ）アクリル酸エステル共重合体としては、例えば（メタ）アクリル酸エステル同士の共重合体、（メタ）アクリル酸エステルと（メタ）アクリル酸エステル以外のモノマーとの共重合体等を用いることができる。また、（メタ）アクリル酸エステルとしては、例えば（メタ）アクリル酸メチル、（メタ）アクリル酸エチル、（メタ）アクリル酸ブチル、（メタ）アクリル酸２−エチルヘキシル及び（メタ）アクリル酸ラウリル等を用いることができる。一方、ポリオキシエチレンアルキルエーテルとしては、例えば化学式Ｒ１−（ＯＣＨ２ＣＨ２）ｎ−ＯＨ（Ｒ１は、炭素数が好ましくは１０〜１６のアルキル基、ｎは好ましくは１〜５の整数）で示される化合物等を用いることができる。具体的には、ポリオキシエチレンラウリルエーテル、ポリオキシエチレンセチルエーテル、ポリオキシエチレンステアリルエーテル、ポリオキシエチレン高級アルコールエーテル、ポリオキシエチレンミリスチルエーテル等である。 As a (meth) acrylic acid ester copolymer, for example, a copolymer of (meth) acrylic acid esters, a copolymer of (meth) acrylic acid ester and a monomer other than (meth) acrylic acid ester, or the like is used. Can do. Examples of the (meth) acrylic acid ester include methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, and lauryl (meth) acrylate. Can be used. On the other hand, as polyoxyethylene alkyl ether, for example, a compound represented by the chemical formula R1- (OCH2CH2) n-OH (R1 is preferably an alkyl group having 10 to 16 carbon atoms, n is preferably an integer of 1 to 5). Etc. can be used. Specific examples include polyoxyethylene lauryl ether, polyoxyethylene cetyl ether, polyoxyethylene stearyl ether, polyoxyethylene higher alcohol ether, polyoxyethylene myristyl ether and the like.
これらのなかでも、（メタ）アクリル酸エステル共重合体としてアクリル酸ブチル共重合体を、またポリオキシエチレンアルキルエーテルとしてポリオキシエチレンラウリルエーテルを選択し、（メタ）アクリル酸エステル共重合体／ポリオキシエチレンアルキルエーテルの質量比が９７／３〜８５／１５とし、アルミナ／シリカの質量比が９７／３〜９０／１０であるアルミナ質繊維と組合せて使用したときに、均質な無機繊維成形体が得られ易く、また容易に嵩密度を小さくすることができる。 Among these, butyl acrylate copolymer is selected as the (meth) acrylic acid ester copolymer, and polyoxyethylene lauryl ether is selected as the polyoxyethylene alkyl ether, and the (meth) acrylic acid ester copolymer / polyester is selected. Homogeneous inorganic fiber molded article when used in combination with alumina fibers having an oxyethylene alkyl ether mass ratio of 97/3 to 85/15 and an alumina / silica mass ratio of 97/3 to 90/10 Can be easily obtained, and the bulk density can be easily reduced.
無機バインダーとしては、例えばシリカゾル、アルミナゾル等が用いられるが、中でもシリカゾルが好ましい。無機バインダーの使用量は、無機繊維成形体の加熱収縮率を低く保持する点から、無機繊維１００質量部に対して２〜１５質量部が好ましく、５〜１０質量部がより好ましい。 As the inorganic binder, for example, silica sol, alumina sol or the like is used, and silica sol is particularly preferable. 2-15 mass parts is preferable with respect to 100 mass parts of inorganic fibers, and, as for the usage-amount of an inorganic binder, the heat shrinkage rate of an inorganic fiber molded object is kept low, 5-10 mass parts is more preferable.
水スラリーの組成の一例を示せば、無機繊維の含有率が０．２〜３．０質量％、有機バインダーが０．０１〜０．３質量％、無機バインダーが０．０１〜０．３質量％、水９５〜９９．７質量％である。なかでも、無機繊維の含有率が０．５〜１．５質量％、有機バインダーが０．０３〜０．１０質量％、無機バインダーが０．０３〜０．１０％、水９８．０〜９９．５質量％であることが好ましい。 If an example of a composition of a water slurry is shown, the content rate of an inorganic fiber will be 0.2-3.0 mass%, an organic binder will be 0.01-0.3 mass%, and an inorganic binder will be 0.01-0.3 mass%. %, And water is 95 to 99.7% by mass. Especially, the content rate of an inorganic fiber is 0.5-1.5 mass%, the organic binder is 0.03-0.10 mass%, the inorganic binder is 0.03-0.10%, and water is 98.0-99. It is preferably 5% by mass.
無機繊維成形体の嵩密度は０．１８ｇ／ｃｍ３以下が好ましく、０．０９〜０．１３ｇ／ｃｍ３がより好ましい。０．１８ｇ／ｃｍ３をこえると空隙率が低くなり、焼成炉の最内層に使用した場合に、繰り返しの急速な加熱、冷却により耐スポーリング性が若干劣ってしまう。嵩密度の調節は、水スラリーの調製時間（混合時間）の調整によって行うことができる。嵩密度は、無機繊維成形体の質量をその体積で除することにより求められる。 The bulk density of the inorganic fiber molded body is preferably 0.18 g / cm 3 or less, and more preferably 0.09 to 0.13 g / cm 3. When it exceeds 0.18 g / cm 3, the porosity becomes low, and when used as the innermost layer of the firing furnace, the spalling resistance is slightly inferior due to repeated rapid heating and cooling. The bulk density can be adjusted by adjusting the preparation time (mixing time) of the water slurry. A bulk density is calculated | required by remove | dividing the mass of an inorganic fiber molded object by the volume.
無機繊維成形体の厚みは２０〜５０ｍｍが好ましい。厚みは、脱型したケーキのプレス圧力の調整によって調節することができる。 The thickness of the inorganic fiber molded body is preferably 20 to 50 mm. The thickness can be adjusted by adjusting the pressing pressure of the demolded cake.
無機繊維成形体は、例えばフェルト、ペーパー、ブロック等に加工し、例えば積層セラミックコンデンサー等の焼成炉の最内層に使用することもできるし、最内層にフェルト、その外側にボードという組み合わせで使用することもできる。 The inorganic fiber molded body can be processed into, for example, felt, paper, block, etc., and can be used as the innermost layer of a firing furnace such as a multilayer ceramic capacitor, or it can be used in combination with felt as the innermost layer and board outside. You can also.
実施例１
オキシ塩化アルミニウム水溶液とシリカゾルとを、アルミナ９７質量％、シリカ３質量％になるように混合し、更にポリビニルアルコールを添加して粘度９００ｍＰａ・ｓの紡糸原液を調製した。これを、円周面に直径０．５ｍｍの孔を３００個設けられてなる直径２５０ｍｍの中空円盤内に入れ、それを回転させて繊維状の紡糸原液を孔から押し出させ、６００℃の熱風により乾燥固化させながらアルミナ質繊維の前躯体を製造した。ついで、トンネル炉にて温度１３５０℃で焼成し、平均繊維径４．０μｍ、アルミナ成分９７質量％、シリカ成分３質量％の無機繊維（アルミナ質繊維）を製造した。
Example 1
An aluminum oxychloride aqueous solution and silica sol were mixed so as to be 97% by mass of alumina and 3% by mass of silica, and polyvinyl alcohol was further added to prepare a spinning dope having a viscosity of 900 mPa · s. This is put in a hollow disk having a diameter of 250 mm in which 300 holes having a diameter of 0.5 mm are provided on the circumferential surface, and rotated to extrude the fibrous spinning dope from the holes, and hot air at 600 ° C. A precursor of alumina fiber was produced while being dried and solidified. Subsequently, it was baked at a temperature of 1350 ° C. in a tunnel furnace to produce inorganic fibers (alumina fibers) having an average fiber diameter of 4.0 μm, an alumina component of 97 mass%, and a silica component of 3 mass%.
このアルミナ質繊維２５６ｇ、無機バインダー（固形分濃度２０質量％のシリカゾル）１８ｇ、有機バインダー３０ｇ、水２５ｋｇ及び硫酸バンド水溶液を適量加え、２０分間湿式混合し、スラリー濃度（アルミナ質繊維、有機バインダー及び無機バインダーの合計含有率）１．０質量％の水スラリーを調製した。この水スラリーを底面網部の寸法が３２０ｍｍ×３２０ｍｍの抄造ボックス（編み目間隔０．５ｍｍ）に流し込み、底面網の下方より吸引により水を抜き、ケーキを製造した。このケーキを脱型後プレスにより厚みを調整した後、１００℃の熱風乾燥機で１６時間乾燥して無機繊維成形体（厚み２５ｍｍのフェルト）を製造し、以下に従う物性を測定した。それらの結果を表１に示す。なお、有機バインダーは、アクリル酸ブチル共重合体４５質量％、ポリオキシエチレンラウリルエーテル３質量％及び水５２質量％からなるエマルジョンであり、ポリオキシエチレンラウリルエーテルは、構造式Ｃ１２Ｈ２５（ＯＣＨ２ＣＨ２）３ＯＨである。 256 g of this alumina fiber, 18 g of an inorganic binder (silica sol having a solid content concentration of 20% by mass), 30 g of an organic binder, 25 kg of water and an aqueous sulfuric acid band solution are added in an appropriate amount and wet mixed for 20 minutes to obtain slurry concentrations (alumina fiber, organic binder and A water slurry having a total content of inorganic binders of 1.0% by mass was prepared. The water slurry was poured into a paper box (bottom spacing 0.5 mm) having a bottom mesh portion size of 320 mm × 320 mm, and water was removed from below the bottom mesh to produce a cake. The cake was demolded and the thickness was adjusted by pressing, and then dried with a hot air dryer at 100 ° C. for 16 hours to produce an inorganic fiber molded body (felt with a thickness of 25 mm). The physical properties were measured as follows. The results are shown in Table 1. The organic binder is an emulsion composed of 45% by mass of a butyl acrylate copolymer, 3% by mass of polyoxyethylene lauryl ether and 52% by mass of water, and the polyoxyethylene lauryl ether has the structural formula C 12 H 25 (OCH it is a 2 CH 2) 3 OH.
（１）嵩密度：フェルトの質量をフェルトの体積で除することにより求めた。
（２）厚み：デプスゲージ（中村製作所社製商品名「ＤＩＧＩ−ＫＡＮＯＮ」）により測定した。
（３）外観：フェルトの表面が均一なものを「良」とし、フェルトの表面に粗い部分が少し見られるものを「可」とし、フェルトの表面が不均一で、所定の形状に成形できないものを「不可」とした。なお、本明細書でこの外観が「良」又は「可」であることを「均質」といっている。
（４）耐アルカリ性外観及び加熱収縮率：フェルトを５０ｍｍ×５０ｍｍに２枚切り出し、その一方をそのままにして静置し（レイヤー置き）、もう一方を長さ方向に３分割し、それぞれ厚み方向を上面に向けた（スタック置き）。表面より５質量％水酸化ナトリウム水溶液６．２５ｇ（３分割の合計量）を含浸させ、１００℃の熱風乾燥機で３時間乾燥した。その後、電気炉で、１４００℃まで加熱し、２４時間保持後室温（２３℃）まで自然冷却するサイクルを８回繰り返した。各サイクルごとに、耐アルカリ性外観を評価し、加熱収縮率の測定を行った。耐アルカリ性外観は目視で評価した。加熱収縮率は、直尺を用いて長さ方向及び厚み方向の寸法を測定し、加熱前の寸法との差を加熱前の寸法で除することにより求めた。
(1) Bulk density: Determined by dividing the mass of the felt by the volume of the felt.
(2) Thickness: Measured with a depth gauge (trade name “DIGI-KANON” manufactured by Nakamura Seisakusho Co., Ltd.).
(3) Appearance: "Fair" means that the felt surface is uniform, and "Yes" means that the felt surface has some rough parts. The felt surface is not uniform and cannot be molded into the specified shape. Was “impossible”. In this specification, the fact that the appearance is “good” or “possible” is referred to as “homogeneous”.
(4) Alkali resistance appearance and heat shrinkage rate: Cut out two pieces of felt into 50 mm x 50 mm, leave one of them as it is (layer placement), divide the other into three in the length direction, Directed to the top (stack placement). From the surface, it was impregnated with 6.25 g of a 5 mass% aqueous sodium hydroxide solution (total amount divided into three parts) and dried with a hot air dryer at 100 ° C. for 3 hours. Then, the cycle which heats to 1400 degreeC with an electric furnace, hold | maintains for 24 hours, and naturally cools to room temperature (23 degreeC) was repeated 8 times. For each cycle, the alkali-resistant appearance was evaluated and the heat shrinkage rate was measured. The alkali resistant appearance was visually evaluated. The heat shrinkage was determined by measuring the length and thickness dimensions using a straight scale and dividing the difference from the dimensions before heating by the dimensions before heating.
なお、紡糸原液粘度は、２０℃粘度をＢ型粘度計（東京計器社製商品名「ＢＨ型」）により測定した。無機繊維の化学組成は、蛍光Ｘ線分析（リガク社製商品名「ＺＳＸ１００ｅ」）により測定した。 In addition, the spinning solution viscosity was measured at 20 ° C. using a B-type viscometer (trade name “BH type” manufactured by Tokyo Keiki Co., Ltd.). The chemical composition of the inorganic fibers was measured by fluorescent X-ray analysis (trade name “ZSX100e” manufactured by Rigaku Corporation).
実施例２〜３
オキシ塩化アルミニウム水溶液とシリカゾルの割合を変え、アルミナ９５質量％、シリカ５質量％のアルミナ質繊維を製造したこと（実施例２）、及びアルミナ９０質量％、シリカ１０質量％のアルミナ質繊維を製造したこと（実施例３）以外は、実施例１と同様に行った。
Examples 2-3
The ratio of aluminum oxychloride aqueous solution and silica sol was changed to produce alumina fiber of 95% alumina and 5% silica by weight (Example 2), and alumina fiber of 90% alumina and 10% silica by weight was produced. The same procedure as in Example 1 was performed except that (Example 3).
実施例４
オキシ塩化アルミニウム水溶液とシリカゾルの割合を変え、アルミナ８０質量％、シリカ２０質量％のアルミナ質繊維を製造したこと、及び水スラリー調整時にアルミナ質繊維を２０５ｇとしたこと以外は、実施例１と同様に行った。
Example 4
The same as in Example 1 except that the ratio of the aluminum oxychloride aqueous solution and silica sol was changed to produce alumina fiber of 80% by mass of alumina and 20% by mass of silica and that the amount of alumina fiber was 205g at the time of water slurry adjustment. Went to.
実施例５
オキシ塩化アルミニウム水溶液とシリカゾルの割合を変え、アルミナ１００質量％のアルミナ質繊維を製造したこと、及び水スラリー調整時にアルミナ質繊維を４６１ｇとしたこと以外は、実施例１と同様に行った。
Example 5
The same procedure as in Example 1 was carried out except that the ratio of the aluminum oxychloride aqueous solution and the silica sol was changed to produce 100% by mass of alumina fiber and that 461 g of alumina fiber was prepared at the time of water slurry adjustment.
比較例１、２
有機系バインダーとして、アクリル酸エステル共重合体のみ（アクリル酸ブチル共重合体４８質量％及び水５２質量％からなるエマルジョン）を用いたこと及び水スラリー調整時にアルミナ質繊維を５１２ｇとしたこと（比較例１）、又はポリオキシエチレンアルキルエーテル（ポリオキシエチレンラウリルエーテル４８質量％及び水５２質量％からなるエマルジョン）のみを用いたこと（比較例２）以外は、実施例１と同様に行った。
Comparative Examples 1 and 2
As an organic binder, only an acrylic ester copolymer (an emulsion composed of 48% by mass of a butyl acrylate copolymer and 52% by mass of water) was used, and the amount of alumina fiber was set to 512 g when adjusting the water slurry (comparison) The same procedure as in Example 1 was carried out except that only Example 1) or polyoxyethylene alkyl ether (an emulsion composed of 48% by mass of polyoxyethylene lauryl ether and 52% by mass of water) was used (Comparative Example 2).
表１から以下のことが分かる。有機バインダーとして、（メタ）アクリル酸エステル共重合体とポリオキシエチレンアルキルエーテルを併用することにより、嵩密度の小さい無機繊維成形体が得られる（実施例１〜５と比較例１，２との対比）。なかでも、無機繊維のアルミナ／シリカの質量比を９７／３〜９０／１０とすることにより、より均質で、嵩密度が小さい無機繊維成形体が得られ、しかも耐アルカリ性を一段と向上させることができた（実施例１〜３）。 Table 1 shows the following. By using a (meth) acrylic acid ester copolymer and polyoxyethylene alkyl ether in combination as the organic binder, an inorganic fiber molded body having a small bulk density is obtained (Examples 1 to 5 and Comparative Examples 1 and 2). Contrast). Among these, by setting the mass ratio of alumina / silica of inorganic fibers to 97/3 to 90/10, an inorganic fiber molded body having a more uniform and low bulk density can be obtained, and the alkali resistance can be further improved. (Examples 1-3).
本発明によって製造された無機繊維成形体は、各種の炉材等として使用することができる。 The inorganic fiber molded body produced by the present invention can be used as various furnace materials.
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