JP2001261465A - Production process of ceramic porous filter - Google Patents
Production process of ceramic porous filterInfo
- Publication number
- JP2001261465A JP2001261465A JP2000073697A JP2000073697A JP2001261465A JP 2001261465 A JP2001261465 A JP 2001261465A JP 2000073697 A JP2000073697 A JP 2000073697A JP 2000073697 A JP2000073697 A JP 2000073697A JP 2001261465 A JP2001261465 A JP 2001261465A
- Authority
- JP
- Japan
- Prior art keywords
- film
- slurry
- porous
- film formation
- porous substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0022—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/00336—Materials with a smooth surface, e.g. obtained by using glass-surfaced moulds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/34—Non-shrinking or non-cracking materials
- C04B2111/343—Crack resistant materials
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】 本発明は、セラミックス多
孔質フィルターの製造方法に係り、更に詳しくは、成膜
用スラリーに特定の有機溶媒を添加するセラミックス多
孔質フィルターの製造方法に関する。TECHNICAL FIELD The present invention relates to a method for manufacturing a ceramic porous filter, and more particularly, to a method for manufacturing a ceramic porous filter in which a specific organic solvent is added to a slurry for film formation.
【０００２】[0002]
【従来の技術】 従来から、多孔質基材上に多孔質膜が
被覆されたセラミックス多孔質フィルターが知られてお
り、水浄化システム等に利用されている。このようなセ
ラミックス多孔質フィルターは、多孔質基材上に多孔質
膜を形成する際に、一般に少なくとも１２００℃以上の
温度で焼結することを必要とする。この方法で得られる
多孔質フィルターは実用上優れた性能を有するが、加熱
温度が比較的高いために経済的、コスト的に問題があ
る。2. Description of the Related Art Conventionally, a ceramic porous filter in which a porous substrate is covered with a porous film has been known, and is used for a water purification system and the like. Such a ceramic porous filter generally requires sintering at a temperature of at least 1200 ° C. when forming a porous film on a porous substrate. Although the porous filter obtained by this method has practically excellent performance, it has economical and cost problems due to the relatively high heating temperature.
【０００３】 そこで、近年になり、より低温度で加熱
焼結する技術が提案されてきており、例えば、特公平６
−６７４６０号公報には、多孔質支持体上に、多孔質で
無機質の分離膜を低温焼結で形成することが記載されて
おり、また、無機材料としてオキシ塩化ジルコニウムを
使用することも開示されている。また、特開平１１−２
３５５０９号公報には、オキシ塩化ジルコニウムをバイ
ンダーとして低温焼結するＺｒＯ2系セラミックス膜が
被覆されたフィルターが開示され、また、膜強度の発現
および膜のクラック防止にはスラリーのｐＨを限られた
範囲に調整しなければならないことが開示されている。[0003] In recent years, techniques for heating and sintering at lower temperatures have been proposed in recent years.
JP-67460 discloses that a porous and inorganic separation membrane is formed on a porous support by low-temperature sintering, and the use of zirconium oxychloride as an inorganic material is also disclosed. ing. Also, JP-A-11-2
Japanese Patent No. 35509 discloses a filter coated with a ZrO 2 -based ceramic film which is sintered at a low temperature using zirconium oxychloride as a binder, and the pH of the slurry is limited in order to develop film strength and prevent cracking of the film. It is disclosed that the range must be adjusted.
【０００４】 さらに、特開平１０−２３５１７２号公
報には、ＺｒＯ2ゾルを使用して低温焼結した膜の開示
があり、”ゾル−ゲル法の科学”（アグネ承風社）の第
２８頁〜第４１頁には、クラックのないゲルバルク体を
作製するために、乾燥の後期に溶液の表面張力が小さく
なるような溶媒を選ぶことが重要であることが開示され
ている。Further, Japanese Patent Application Laid-Open No. Hei 10-235172 discloses a film sintered at a low temperature using a ZrO 2 sol, and is described in “Sol-Gel Method Science” (Agne Shofu), page 28. Pp. 41 to 41 disclose that it is important to select a solvent that reduces the surface tension of the solution in the latter half of drying in order to produce a gel bulk without cracks.
【０００５】[0005]
【発明が解決しようとする課題】 しかしながら、上記
したオキシ塩化ジルコニウムを使用する低温焼結膜にお
いては、乾燥時にクラックが発生しやすいため、乾燥速
度を相当遅くする必要がある。また、膜へのクラック防
止のためには、スラリーｐＨの厳密な制御が必要であ
る。さらに、成膜後の膜の表面が粗く、水浄化システム
に適用した場合、膜面に堆積した汚泥等を除去しにくく
なり、いわゆるファウリングしやすい膜になってしまう
という問題がある。However, in the low-temperature sintering film using zirconium oxychloride described above, cracks are apt to occur during drying, so that the drying speed needs to be considerably reduced. In addition, strict control of the slurry pH is required to prevent cracks in the film. Furthermore, when the film is rough, the surface of the film is rough, and when applied to a water purification system, there is a problem that it is difficult to remove sludge and the like deposited on the film surface, resulting in a film that is easily fouled.
【０００６】 したがって、本発明は上記した従来技術
の課題を解決するためになされたもので、その目的とす
るところは、多孔質基材上に多孔質膜を低温焼結で被覆
するに当たり、膜の乾燥速度を速く、またスラリーのｐ
Ｈを制御することなく、成膜後の膜表面の平滑度に優
れ、しかも、多孔質膜にクラックが発生しないセラミッ
クス多孔質フィルターの製造方法を提供することにあ
る。Accordingly, the present invention has been made to solve the above-mentioned problems of the prior art, and an object of the present invention is to provide a method for coating a porous film on a porous substrate by low-temperature sintering. Drying speed and slurry p
An object of the present invention is to provide a method for producing a ceramic porous filter which is excellent in smoothness of a film surface after film formation without controlling H and which does not cause cracks in a porous film.
【０００７】[0007]
【課題を解決するための手段】 即ち、本発明によれ
ば、オキシ塩化ジルコニウムを出発原料とし熱処理によ
りＺｒＯ2になるものを骨材粒子の結合材として使用
し、該骨材粒子と該結合材を含有する成膜用スラリーを
形成した後、該成膜用スラリーを多孔質基材上に付着さ
せて層を形成し、次いで熱処理することにより、多孔質
基材上にセラミックス膜を形成するセラミックス多孔質
フィルターの製造方法において、前記成膜用スラリー
に、水より高沸点でかつ低表面張力の水溶性の有機溶媒
を添加することを特徴とするセラミックス多孔質フィル
ターの製造方法、が提供される。That is, according to the present invention, zirconium oxychloride is used as a starting material, and a material which becomes ZrO 2 by heat treatment is used as a binder for the aggregate particles, and the aggregate particles and the binder are used. After forming a film-forming slurry containing, the film-forming slurry is deposited on a porous substrate to form a layer, and then heat-treated to form a ceramic film on the porous substrate. In the method for producing a porous filter, a method for producing a ceramic porous filter is provided, wherein a water-soluble organic solvent having a higher boiling point than water and a low surface tension is added to the slurry for film formation. .
【０００８】 上記の製造方法においては、用いる有機
溶媒が、ジメチルフォルムアミド（ＤＭＦ）であること
が望ましい。In the above-mentioned production method, it is desirable that the organic solvent used is dimethylformamide (DMF).
【０００９】[0009]
【発明の実施の形態】 以下、本発明を詳しく説明す
る。本発明では、オキシ塩化ジルコニウムを出発原料と
し、熱処理によりＺｒＯ2になるものを骨材粒子の結合
材として使用する。そして、この結合材と骨材粒子を混
合して成膜用スラリーを形成した後、この成膜用スラリ
ーを多孔質基材上に付着させて被覆層を形成する。次い
で、この被覆層を低温にて熱処理することにより、多孔
質基材上にセラミックス膜を形成することにより、セラ
ミックス多孔質フィルターを製造する方法である。そし
て、本発明においては、成膜用スラリーに、水より高沸
点でかつ低表面張力の水溶性の有機溶媒を添加すること
に特徴を有する。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail. In the present invention, zirconium oxychloride is used as a starting material, and a material that becomes ZrO 2 by heat treatment is used as a binder for aggregate particles. Then, after the binder and the aggregate particles are mixed to form a slurry for film formation, the slurry for film formation is adhered to a porous substrate to form a coating layer. Next, this coating layer is subjected to a heat treatment at a low temperature to form a ceramic film on the porous substrate, thereby producing a ceramic porous filter. The present invention is characterized in that a water-soluble organic solvent having a higher boiling point than water and a low surface tension is added to the slurry for film formation.
【００１０】 本発明では、このような特定の有機溶媒
を成膜用スラリーに添加することにより、スラリーのｐ
Ｈを特に制御せず、膜の乾燥速度を速くして、多孔質基
材上に被覆層を形成することができる。しかも、多孔質
膜の膜表面は平滑度に優れ、クラックが発生しないセラ
ミックス多孔質フィルターを得ることができる。In the present invention, by adding such a specific organic solvent to the slurry for film formation, the p of the slurry is reduced.
The coating layer can be formed on the porous substrate by increasing the drying rate of the film without controlling H in particular. Moreover, the surface of the porous film has excellent smoothness, and a ceramic porous filter free from cracks can be obtained.
【００１１】 本発明で用いる水より高沸点でかつ低表
面張力の水溶性の有機溶媒としては、酢酸、エチレング
リコール、フォルムアミド、ジメチルフォルムアミド
（ＤＭＦ）等が使用できるが、特に、ＤＭＦは、得られ
る多孔質膜表面の平滑性、膜強度の点で優れており、特
に好ましい。As the water-soluble organic solvent having a higher boiling point and lower surface tension than water used in the present invention, acetic acid, ethylene glycol, formamide, dimethylformamide (DMF) and the like can be used. The surface of the obtained porous membrane is excellent in terms of smoothness and membrane strength, and is particularly preferable.
【００１２】 成膜用スラリーに添加する有機溶媒の添
加量は、水に対して３〜２０重量％であることが好まし
い。添加量が３重量％未満では、得られる多孔質膜の表
面が凸凹になるほか、膜にクラックも発生することがあ
る。一方、添加量が２０重量％より多いと膜結合不良に
なることがある。The amount of the organic solvent added to the film forming slurry is preferably 3 to 20% by weight based on water. When the addition amount is less than 3% by weight, the surface of the obtained porous film becomes uneven, and cracks may be generated in the film. On the other hand, if the addition amount is more than 20% by weight, poor film bonding may occur.
【００１３】 本発明において、セラミック多孔質膜に
使用する骨材粒子としては特に限定されず、Ａｌ2Ｏ3、
ＺｒＯ2、ＴｉＯ2、Ａｌ2Ｏ3・ＳｉＯ2（ムライト）等
が適用できる。もちろんこれらの混合物等も適用でき
る。また、その平均粒子径は０．１〜１０μｍの範囲と
することが望ましい。In the present invention, the aggregate particles used for the ceramic porous membrane are not particularly limited, and Al 2 O 3 ,
ZrO 2 , TiO 2 , Al 2 O 3 .SiO 2 (mullite) and the like can be applied. Needless to say, a mixture thereof can be applied. Further, the average particle diameter is desirably in the range of 0.1 to 10 μm.
【００１４】 次に、多孔質膜が被覆される多孔質基材
としては、多孔質のセラミックスからなるもので、その
材質としては、Ａｌ2Ｏ3、ＺｒＯ2、ＴｉＯ2、Ａｌ2Ｏ3
・ＳｉＯ2（ムライト）等が適用でき、特に限定はされ
ない。また、多孔質基材の形状も特に限定はなく、平板
状、円筒状およびハニカム状等に適用できる。Next, the porous substrate to be coated with the porous film is made of porous ceramics, and is made of Al 2 O 3 , ZrO 2 , TiO 2 , Al 2 O 3
-SiO 2 (mullite) or the like can be applied, and there is no particular limitation. The shape of the porous substrate is not particularly limited, and can be applied to a flat plate shape, a cylindrical shape, a honeycomb shape, or the like.
【００１５】 なお、成膜用スラリーには、必要に応じ
て分散剤や成形用の有機バインダーを適宜添加しても構
わない。また、多孔質基材上へ成膜用スラリーを被覆す
る成膜方法としては、特に限定されないが、ディッピン
グ法や濾過成膜法等が好ましく適用することができる。Note that a dispersant and an organic binder for molding may be appropriately added to the slurry for film formation, if necessary. Further, a film forming method for coating the film forming slurry on the porous substrate is not particularly limited, but a dipping method, a filtration film forming method, or the like can be preferably applied.
【００１６】 本発明は、オキシ塩化ジルコニウムを出
発原料とし、熱処理によりＺｒＯ2になるものを結合材
として用いており、したがって、成膜用スラリーを多孔
質基材上に付着させた後の熱処理は、オキシ塩化ジルコ
ニウムがＺｒＯ2に転換する温度である４５０〜６００
℃で行われる。より好ましい熱処理温度は、４５０〜５
５０℃である。In the present invention, zirconium oxychloride is used as a starting material, and a material that becomes ZrO 2 by heat treatment is used as a binder. Therefore, heat treatment after depositing a slurry for film formation on a porous base material is not required. , 450-600 zirconium oxychloride is a temperature that converts the ZrO 2
Performed at ° C. A more preferred heat treatment temperature is 450 to 5
50 ° C.
【００１７】[0017]
【実施例】 次に、本発明を実施例により更に具体的に
説明する。 （実施例１〜１４、比較例１〜７）下記の条件で、Ａｌ
2Ｏ3からなる多孔質基材表面上にセラミックス多孔質膜
を形成した。Next, the present invention will be described more specifically with reference to examples. (Examples 1 to 14, Comparative Examples 1 to 7) Under the following conditions, Al
A ceramic porous film was formed on the surface of a porous substrate made of 2 O 3 .
【００１８】多孔質基材チューブ状多孔質基材 Ａｌ2Ｏ3粒子からなり、水銀圧入法で測定した平均細孔
径が１０μｍで、外径１０ｍｍ、内径７ｍｍ、長さ１０
００ｍｍの円筒状のものを用いた。Porous substrate Tubular porous substrate consisting of Al 2 O 3 particles, having an average pore diameter of 10 μm measured by a mercury intrusion method, an outer diameter of 10 mm, an inner diameter of 7 mm, and a length of 10 μm.
A 00 mm cylindrical shape was used.
【００１９】多孔質膜の作製 (1)成膜用スラリー調製 作製法： ・混合物Ａ：表１に示すように、水、添加溶媒、及び骨
材を混合して混合物Ａとした。 ・混合物２：ウェランガム、オキシ塩化ジルコニウムを
水に溶解して混合物Ｂとした。 この混合物Ａと混合物Ｂを混合して、成膜用スラリーと
した。尚、骨材濃度（骨材／スラリー）は、骨材粒径が
１μｍ以下では３重量％、それを超える場合には１０重
量％とした。Preparation of Porous Film (1) Preparation of Slurry for Film Formation Preparation Method: Mixture A: As shown in Table 1, water, an additive solvent, and an aggregate were mixed to obtain a mixture A. -Mixture 2: Welan gum and zirconium oxychloride were dissolved in water to obtain a mixture B. The mixture A and the mixture B were mixed to form a slurry for film formation. The aggregate concentration (aggregate / slurry) was 3% by weight when the aggregate particle size was 1 μm or less, and 10% by weight when the aggregate particle size exceeded 3 μm.
【００２０】(2)濾過成膜 成膜方法としては、濾過成膜法を採用し、図１に示すよ
うな真空チャンバ６、貯蔵槽８、スラリーポンプ７、フ
ランジ２，３、配管１０等からなる装置により実施し
た。(2) Filtration film formation As a film formation method, a filter film formation method is adopted, and the film formation is performed from a vacuum chamber 6, a storage tank 8, a slurry pump 7, flanges 2, 3, pipes 10 and the like as shown in FIG. It was carried out by the following device.
【００２１】 多孔質基材１は、多孔質基材１の外周面
側と貫通孔１７内部とが気密的に隔離されるように貫通
孔１７の両開口端をＯ−リング４、フランジ２，３、ボ
ルト５により固定した後、貯蔵槽８内のスラリー９をス
ラリーポンプ７により２Ｋｇ／ｃｍ2の吐出圧で貫通孔
１７内に３０秒間連続的に送液した。なお、多孔質基材
１に成膜されず貫通孔１７内を通過したスラリー９は、
配管１０を通過して貯蔵槽８に循環される。１１，１４
はバルブで、１３が減圧機である。The porous substrate 1 has both open ends of the through-hole 17 with the O-ring 4, the flange 2, and the flange 2, such that the outer peripheral surface side of the porous substrate 1 and the inside of the through-hole 17 are hermetically isolated. 3. After fixing with the bolts 5, the slurry 9 in the storage tank 8 was continuously fed into the through-hole 17 by the slurry pump 7 at a discharge pressure of 2 kg / cm 2 for 30 seconds. The slurry 9 that has passed through the through hole 17 without being formed on the porous substrate 1 is
It is circulated through the pipe 10 to the storage tank 8. 11,14
Is a valve, and 13 is a decompressor.
【００２２】 その後、スラリー９の送液を継続しなが
ら真空チャンバ６内を０．１ａｔｍ以下の真空条件と
し、多孔質基材１の外周面側と貫通孔１７内部との間に
濾過差圧を付与することにより、貫通孔１７内のスラリ
ーを多孔質基材１の外周面側から減圧吸引し成膜を行っ
た。この場合における濾過差圧は、圧力計１５で示され
る貫通孔１７内のスラリー９の圧力と圧力計１６で示さ
れる真空チャンバ６内の雰囲気圧力との差圧となる。Thereafter, the vacuum pressure in the vacuum chamber 6 is set to 0.1 atm or less while the slurry 9 is continuously supplied, and a filtration pressure difference between the outer peripheral surface side of the porous substrate 1 and the inside of the through hole 17 is increased. By applying the slurry, the slurry in the through-hole 17 was suctioned from the outer peripheral surface side of the porous substrate 1 under reduced pressure to form a film. In this case, the filtration pressure difference is the pressure difference between the pressure of the slurry 9 in the through hole 17 indicated by the pressure gauge 15 and the atmospheric pressure in the vacuum chamber 6 indicated by the pressure gauge 16.
【００２３】 成膜終了後、貫通孔１７内の遊離のスラ
リーを排出し、０．１ａｔｍ以下の真空条件で減圧吸引
を継続することにより、成膜層及び基材細孔内に含まれ
る水分を減圧脱水し、成膜体とした。After the completion of the film formation, the free slurry in the through-hole 17 is discharged, and the vacuum contained under the vacuum condition of 0.1 atm or less is continued to reduce the moisture contained in the film formation layer and the base material pores. It was dehydrated under reduced pressure to obtain a film.
【００２４】乾燥 上記のようにして多孔質基材上にスラリーを成膜した
後、８０℃にて乾燥した。 焼成 乾燥後、大気処理用の電気炉を使用し、温度５５０℃で
４時間熱処理（焼成）した。Drying After forming a slurry on the porous substrate as described above, the slurry was dried at 80 ° C. Firing After drying, heat treatment (firing) was performed at a temperature of 550 ° C. for 4 hours using an electric furnace for air treatment.
【００２５】膜表面平滑性評価 得られたセラミックス多孔質膜について、以下のように
その評価を行った。膜の表面粗さ：試料の上部、中央、
下部について、骨材粒径の１００倍長さ部分について、
膜の骨材粒径の５倍以上の凸凹箇所の数を測定し、５以
下が◎、６−１０が○、１１以上は×とした。Evaluation of Film Surface Smoothness The obtained ceramic porous film was evaluated as follows. Surface roughness of the film: top, center,
For the lower part, about 100 times the length of the aggregate particle size,
The number of irregularities at least 5 times the aggregate particle diameter of the membrane was measured, and 、 ５ was given for 5 or less, ○ for 6-10, and × for 11 or more.
【００２６】・膜内クラックの有無：試料長手方向に２
０分割し、その各々の任意の領域（５００μｍ四方）を
走査型顕微鏡にて観察し、長さ５０μｍ以上のクラック
の有無を調べた。 ・膜結合状態：膜表面にセロファンテープを張りつけ、
剥がした時の膜の剥がれ具合で評価した。剥がれがない
場合を○、剥がれが生じた時を×とした。得られた結果
を表１に示す。The presence or absence of cracks in the film: 2 in the longitudinal direction of the sample
The sample was divided into 0 parts, and each of the areas (500 μm square) was observed with a scanning microscope to check for cracks having a length of 50 μm or more.・ Membrane bonding state: Cellophane tape is stuck on the membrane surface,
Evaluation was made on the degree of peeling of the film when peeled. The case where there was no peeling was evaluated as ○, and the case where peeling occurred was evaluated as x. Table 1 shows the obtained results.
【００２７】[0027]
【表１】 [Table 1]
【００２８】 表１において、＊１〜＊６は以下の意味
を示す。 *1. レーサ゛ー回折式粒度測定装置で測定し、その50%径値。 *2. シ゛ルコニア換算量／水×100 *3. DMF:シ゛メチルフォルムアミト゛、EG:エチレンク゛リコール、FA:フォルムアミト゛ *4. 添加溶媒量／水×100 *5. 80℃での乾燥時間 *6. 昇温速度も制御し、0.1℃/minで80℃まで昇温した
後、保持。 又、表１において、比１は比較例１のことで、同様に、
比２から比７は、比較例２から７を示す。In Table 1, * 1 to * 6 have the following meanings. * 1. 50% diameter value measured with a laser diffraction particle size analyzer. * 2. Sirconia conversion amount / water x 100 * 3. DMF: methyl formamide, EG: ethylene glycol, FA: formamide * 4. Additive solvent amount / water x 100 * 5. Drying time at 80 ° C * 6. The rate of temperature rise is also controlled, and after the temperature is raised to 80 ° C at 0.1 ° C / min, it is maintained. Also, in Table 1, the ratio 1 is Comparative Example 1, and similarly,
Ratios 2 to 7 indicate Comparative Examples 2 to 7.
【００２９】（考察）実施例１〜６、１３および１４よ
り、種々の材質の骨材、骨材粒径に対し適用できること
が確認された。添加溶媒のない比較例１〜３では膜表面
平滑性も悪く、乾燥時間も長くしなければならないこと
が分かった。また、実施例１〜６より、膜表面平滑性の
点で、ＤＭＦが優れていることがわかる。実施例７〜１
４及び比較例４〜７より、ＤＭＦが３重量％未満では効
果がなく、２０重量％より多いと膜結合不良を起こすこ
とがわかる。(Consideration) From Examples 1 to 6, 13 and 14, it was confirmed that the present invention can be applied to aggregates of various materials and aggregate particle sizes. In Comparative Examples 1 to 3 having no added solvent, it was found that the film surface smoothness was poor and the drying time had to be increased. Further, it can be seen from Examples 1 to 6 that DMF is excellent in terms of film surface smoothness. Examples 7-1
4 and Comparative Examples 4 to 7, it is understood that there is no effect when DMF is less than 3% by weight, and that when DMF is more than 20% by weight, poor film bonding occurs.
【００３０】[0030]
【発明の効果】 以上説明したように、本発明によれ
ば、スラリーのｐＨを特に制御せず、膜の乾燥速度を速
くして、多孔質基材上に被覆層を形成することができ
る。しかも、多孔質膜の膜表面は平滑度に優れ、クラッ
クが発生しないセラミックス多孔質フィルターを得るこ
とができる。As described above, according to the present invention, a coating layer can be formed on a porous substrate by increasing the drying speed of a film without particularly controlling the pH of a slurry. Moreover, the surface of the porous film has excellent smoothness, and a ceramic porous filter free from cracks can be obtained.
【図１】 濾過成膜法に使用する装置の例を示す概略図
である。FIG. 1 is a schematic view showing an example of an apparatus used for a filtration film formation method.
【符号の説明】 １…多孔質基材、２，３…フランジ、４…Ｏ−リング、
５…ボルト、６…真空チャンバ、７…スラリーポンプ、
８…貯蔵槽、９…スラリー、１０…配管、１１，１４…
バルブ、１３…減圧機、１５，１６…圧力計、１７…貫
通孔。[Description of Signs] 1 ... porous base material, 2,3 ... flange, 4 ... O-ring,
5 bolt, 6 vacuum chamber, 7 slurry pump,
8 ... storage tank, 9 ... slurry, 10 ... piping, 11, 14 ...
Valves, 13: pressure reducer, 15, 16: pressure gauge, 17: through hole.
Claims (2)
熱処理によりＺｒＯ2になるものを骨材粒子の結合材と
して使用し、該骨材粒子と該結合材を含有する成膜用ス
ラリーを形成した後、該成膜用スラリーを多孔質基材上
に付着させて層を形成し、次いで熱処理することによ
り、多孔質基材上にセラミックス膜を形成するセラミッ
クス多孔質フィルターの製造方法において、 前記成膜用スラリーに、水より高沸点でかつ低表面張力
の水溶性の有機溶媒を添加することを特徴とするセラミ
ックス多孔質フィルターの製造方法。1. A method of forming zirconium oxychloride as a starting material, which becomes ZrO 2 by heat treatment as a binder for aggregate particles, and forming a slurry for film formation containing the aggregate particles and the binder, The method for producing a ceramic porous filter, wherein a ceramic film is formed on a porous substrate by forming a layer by attaching the slurry for film formation on a porous substrate and then performing a heat treatment, A method for producing a ceramic porous filter, comprising adding a water-soluble organic solvent having a higher boiling point and lower surface tension than water to a slurry.
ある請求項１記載のセラミックス多孔質フィルターの製
造方法。2. The method according to claim 1, wherein the organic solvent is dimethylformamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000073697A JP2001261465A (en) | 2000-03-16 | 2000-03-16 | Production process of ceramic porous filter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000073697A JP2001261465A (en) | 2000-03-16 | 2000-03-16 | Production process of ceramic porous filter |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001261465A true JP2001261465A (en) | 2001-09-26 |
Family
ID=18591903
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000073697A Withdrawn JP2001261465A (en) | 2000-03-16 | 2000-03-16 | Production process of ceramic porous filter |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001261465A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6447599B1 (en) * | 2000-09-13 | 2002-09-10 | Compagnie Du Sol | Method of limiting the release of organic materials into the environment during the making of foundations, and concrete which can be used in said method |
| EP1666220A1 (en) * | 2003-09-19 | 2006-06-07 | Ngk Insulators, Ltd. | Method for producing ceramic sintered article, ceramic sintered article and light emitting container |
| WO2007094267A1 (en) * | 2006-02-16 | 2007-08-23 | Ngk Insulators, Ltd. | Process for producing ceramic porous membrane |
| JP2007254222A (en) * | 2006-03-24 | 2007-10-04 | Ngk Insulators Ltd | Porous ceramic film, ceramic filter and its manufacturing method |
| JP2010506699A (en) * | 2006-10-18 | 2010-03-04 | 日本碍子株式会社 | Method for producing ceramic porous membrane and method for producing ceramic filter |
| US10121652B1 (en) * | 2017-06-07 | 2018-11-06 | Nxp Usa, Inc. | Formation of metal oxide layer |
| CN112939580A (en) * | 2021-01-29 | 2021-06-11 | 广西碧清源环保投资有限公司 | Preparation method of ceramic filtering membrane |
-
2000
- 2000-03-16 JP JP2000073697A patent/JP2001261465A/en not_active Withdrawn
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6447599B1 (en) * | 2000-09-13 | 2002-09-10 | Compagnie Du Sol | Method of limiting the release of organic materials into the environment during the making of foundations, and concrete which can be used in said method |
| EP1666220A1 (en) * | 2003-09-19 | 2006-06-07 | Ngk Insulators, Ltd. | Method for producing ceramic sintered article, ceramic sintered article and light emitting container |
| EP1666220A4 (en) * | 2003-09-19 | 2008-12-17 | Ngk Insulators Ltd | Method for producing ceramic sintered article, ceramic sintered article and light emitting container |
| WO2007094267A1 (en) * | 2006-02-16 | 2007-08-23 | Ngk Insulators, Ltd. | Process for producing ceramic porous membrane |
| US7608298B2 (en) | 2006-02-16 | 2009-10-27 | Ngk Insulators, Ltd. | Method of manufacturing ceramic porous membrane |
| JP2007254222A (en) * | 2006-03-24 | 2007-10-04 | Ngk Insulators Ltd | Porous ceramic film, ceramic filter and its manufacturing method |
| JP2010506699A (en) * | 2006-10-18 | 2010-03-04 | 日本碍子株式会社 | Method for producing ceramic porous membrane and method for producing ceramic filter |
| US10121652B1 (en) * | 2017-06-07 | 2018-11-06 | Nxp Usa, Inc. | Formation of metal oxide layer |
| CN112939580A (en) * | 2021-01-29 | 2021-06-11 | 广西碧清源环保投资有限公司 | Preparation method of ceramic filtering membrane |
| CN112939580B (en) * | 2021-01-29 | 2022-07-01 | 广西碧清源环保投资有限公司 | Preparation method of ceramic filtering membrane |
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