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Publication number
JP2713198B2
JP2713198B2 JP7000694A JP69495A JP2713198B2 JP 2713198 B2 JP2713198 B2 JP 2713198B2 JP 7000694 A JP7000694 A JP 7000694A JP 69495 A JP69495 A JP 69495A JP 2713198 B2 JP2713198 B2 JP 2713198B2
Authority
JP
Japan
Prior art keywords
filter
filter according
yarn
bobbin
terephthalic acid
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.)
Expired - Lifetime
Application number
JP7000694A
Other languages
Japanese (ja)
Other versions
JPH07284618A (en
Inventor
暎二 田原
信夫 福田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Chemical Corp
Original Assignee
Mitsubishi Chemical Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
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Application filed by Mitsubishi Chemical Corp filed Critical Mitsubishi Chemical Corp
Priority to JP7000694A priority Critical patent/JP2713198B2/en
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Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/52Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Filtering Materials (AREA)
  • Catalysts (AREA)

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明はフィルターに関する。詳
しくは溶液から固形異物を除去するための溶液濾過用フ
ィルターに関する。
The present invention relates to filters. More specifically, the present invention relates to a solution filtration filter for removing solid foreign matter from a solution.

【0002】[0002]

【従来の技術】溶液から固形異物を除去する用途は多く
存在する。例えば、テレフタル酸は、通常パラキシレン
の液相酸化によって製造される。しかしながら、ポリエ
ステル等の製品にしたときの着色の原因である4−カル
ボキシベンズアルデヒド等の不純物を多く含むものであ
りこれを除去することが望ましい。従って、一般に、粗
製テレフタル酸の水溶液を200〜400℃の高温で、
貴金属含有触媒の存在下、接触処理または水素添加処理
を行なう。該精製処理後には、触媒の微粉粒子等の固形
異物が含まれるので、これを除去するために、テレフタ
ル酸水溶液を濾過する必要がある。
BACKGROUND OF THE INVENTION There are many uses for removing solid foreign matter from solutions. For example, terephthalic acid is usually produced by liquid phase oxidation of para-xylene. However, it contains a large amount of impurities such as 4-carboxybenzaldehyde, which cause coloring in products such as polyester, and it is desirable to remove these. Therefore, generally, an aqueous solution of crude terephthalic acid is heated at a high temperature of 200 to 400 ° C.
The contact treatment or the hydrogenation treatment is performed in the presence of the noble metal-containing catalyst. After the purification treatment, solid foreign substances such as fine powder particles of the catalyst are contained. Therefore, it is necessary to filter the terephthalic acid aqueous solution in order to remove the foreign substances.

【0003】上記精製処理後のテレフタル酸水溶液は、
高温かつ高腐蝕性であるので、従来、焼結チタン等の金
属材料または多孔性炭素床等を濾過材として使用してい
た(特公昭51−32618)。
[0003] The terephthalic acid aqueous solution after the above purification treatment is
Conventionally, a metal material such as sintered titanium or a porous carbon bed or the like has been used as a filtering material because of its high temperature and high corrosiveness (Japanese Patent Publication No. 51-32618).

【0004】[0004]

【発明が解決しようとする課題】しかしながら、金属材
料を濾過材とした場合、耐蝕性、機械的強度の問題があ
る。また、上記の濾過材を用いた場合、従来、粒径が2
0μm程度以下の特に微細な粒子の除去が充分ではなか
った。該微細粒子がテレフタル酸に混入した場合の問題
としては、例えばテレフタル酸よりポリエステルを製造
し繊維とした場合の糸切れ、フィルムとした場合のフィ
ルム表面の白化等のトラブルの原因のひとつとなること
が考えられる。以上のように溶液から固形異物を除去す
る場合、特に上記のテレフタル酸水溶液のような高温か
つ高腐蝕性の溶液においては、これに充分適用できる溶
液濾過用フィルターが望まれていた。
However, when a metal material is used as a filtering material, there are problems of corrosion resistance and mechanical strength. In addition, when the above-mentioned filtering material is used, conventionally, the particle size is 2
Removal of particularly fine particles of about 0 μm or less was not sufficient. As a problem when the fine particles are mixed into terephthalic acid, for example, it is one of the causes of troubles such as thread breakage when a polyester is produced from terephthalic acid and used as a fiber, and whitening of the film surface when a film is used. Can be considered. As described above, in the case of removing solid foreign matter from a solution, especially for a high-temperature and highly corrosive solution such as the above-mentioned terephthalic acid aqueous solution, a solution filtration filter which can be sufficiently applied to the solution has been desired.

【0005】[0005]

【課題を解決するための手段】本発明者等は上記実情に
鑑み、高温かつ高腐蝕性の溶液中の微細の固形異物を効
率よく除去する方法について種々検討した結果、濾過材
としてカーボンファイバーを用いた特定構造の糸巻きタ
イプのフィルターを用いることが適当であることを見い
出し、本発明に到達した。
In view of the above circumstances, the present inventors have conducted various studies on a method for efficiently removing fine solid foreign matter in a high-temperature and highly corrosive solution. The present inventors have found that it is appropriate to use a thread-wound type filter having the specific structure used, and have reached the present invention.

【0006】すなわち、本発明の要旨は、少なくとも一
端が開放された孔を有するボビンの側面をカーボンファ
イバー・マルチフィラメントの撚糸で巻回被覆してなる
フィルターに存する。
[0006] That is, the gist of the present invention resides in a filter in which at least one side of a bobbin having a hole opened at one end is wound and covered with a twisted carbon fiber multifilament yarn.

【0007】以下、本発明につき詳細に説明する。本発
明のフィルターを図面を用いながら説明するに、図1
は、本発明のフィルターの1例を示す全体斜視図、図2
は図1のフィルターの断面図である。このフィルターは
通常、1対のフランジ2,2′と、穿孔5を有するボビ
ン1から構成され、上記フランジ2,2′の間に位置す
るボビン1上に巻線3が施されている。
Hereinafter, the present invention will be described in detail. The filter of the present invention will be described with reference to the drawings.
FIG. 2 is an overall perspective view showing an example of the filter of the present invention, and FIG.
2 is a cross-sectional view of the filter of FIG. This filter usually comprises a pair of flanges 2, 2 'and a bobbin 1 having a perforation 5, and a winding 3 is provided on the bobbin 1 located between the flanges 2, 2'.

【0008】巻線3は、カーボンファイバー(フィラメ
ント単糸径は通常1〜20μm、好ましくは5〜10μ
m)の短糸で、通常、長さが1〜100mm、好ましく
は5〜30mmのものを紬いで糸状(マルチフィラメン
ト)とし、その紬糸径が通常0.2〜5mm、好ましく
は1〜3mmとなるようにして、更に該紬糸を、通常2
〜5本撚り合わせて、通常2〜10mm径とした太糸で
ある。また、巻線3は、前記の短糸と同じフィラメント
単糸径の連続糸を通常50〜1000本集束し、適度に
ねじりを加えてマルチフィラメントとし、更にこれを、
通常2〜10本撚り合わせたものでもよい。該太糸は、
通常の方法で巻回し、ボビン1を好ましくは完全に覆
い、密接した均一の巻線の分布を与えるようにし、巻き
厚は、通常0.5〜5cm、好ましくは1 〜3cmとす
る。また、密接した均一の巻線の分布を得るためには、
綾角を10〜20°とするのが好ましい。
The winding 3 is made of carbon fiber (filament single yarn diameter is usually 1 to 20 μm, preferably 5 to 10 μm
m) The short yarn having a length of usually 1 to 100 mm, preferably 5 to 30 mm is formed into a thread form (multifilament), and the pongee yarn diameter is usually 0.2 to 5 mm, preferably 1 to 3 mm. So that the pongee yarn is usually 2
It is a thick yarn having a diameter of usually 2 to 10 mm by twisting up to 5 strands. In addition, the winding 3 usually bundles 50 to 1000 continuous yarns having the same filament single yarn diameter as the short yarn, and twists the yarn appropriately to form a multifilament.
Usually, two to ten strands may be used. The thick thread is
It is wound in the usual way, preferably covering the bobbin 1 completely, so as to give a close and even distribution of the windings, the winding thickness is usually 0.5-5 cm, preferably 1-3 cm. Also, to obtain a close and even distribution of windings,
The helix angle is preferably set to 10 to 20 °.

【0009】上記の構成を採用することにより、同じカ
ーボンファイバーを素材とした不織布等と比較して、カ
ーボンファイバーの充てん状態が著しく緻密となる。フ
ィルターの実際の使用方法としては、ボビン1の空胴4
より溶液を供給することも可能であるが、好ましくは、
巻線3の外側から溶液を供給し、空胴4より処理液を取
り出す方法が採用される。
By adopting the above-mentioned structure, the filled state of the carbon fiber becomes extremely dense as compared with a nonwoven fabric or the like using the same carbon fiber as a material. The actual use of the filter is as follows.
It is possible to supply more solution, but preferably
A method of supplying a solution from the outside of the winding 3 and taking out the processing liquid from the cavity 4 is adopted.

【0010】本発明のフィルターの処理対象となる溶液
の種類は特に限定されるものではないが、前記のテレフ
タル酸水溶液のような高温かつ高腐蝕性の溶液において
好適である。テレフタル酸は、通常、分子状酸素を用い
るパラキシレンの液相酸化によって製造される。これに
より得られた粗製テレフタル酸は、通常、重量基準で1
00〜10,000ppmの不純物、例えば、4−カル
ボキシベンズアルデヒド、P−トルイル酸等を含む。こ
れら不純物は、テレフタル酸を原料としてポリエステル
等の製品にしたときの着色の原因となるのでこれをでき
るだけ除去することが望ましい。従って、一般に、粗製
テレフタル酸の水溶液を200〜400℃の高温で、貴
金属含有触媒の存在下、接触処理または水素添加処理し
て精製を行う。該処理方法としては、通常200〜40
0℃の温度で、貴金属触媒の存在下で、通常、水素を導
入して行なわれる。貴金属源としては、パラジウム、ル
テニウム、ロジウム、オスミウム、イリジウム、白金等
あるいはこれらの金属酸化物から選ばれる。これらの金
属もしくは金属酸化物は触媒としてそのまま使用するこ
ともできるが、活性炭のごとき担体に担持したものが特
に有効である。以上の接触処理は、連続法あるいは回分
法の何れにも適用できるが、特に連続法に適している。
該処理後のテレフタル酸水溶液を濾過するフィルターと
して、本発明のフィルターが適当である。
The type of solution to be treated by the filter of the present invention is not particularly limited, but is suitable for a high-temperature and highly corrosive solution such as the above-mentioned terephthalic acid aqueous solution. Terephthalic acid is usually produced by liquid phase oxidation of para-xylene using molecular oxygen. The crude terephthalic acid obtained in this way is usually 1% by weight.
It contains from 00 to 10,000 ppm of impurities such as 4-carboxybenzaldehyde, P-toluic acid and the like. Since these impurities cause coloring when a product such as polyester is made from terephthalic acid as a raw material, it is desirable to remove them as much as possible. Therefore, generally, an aqueous solution of crude terephthalic acid is subjected to contact treatment or hydrogenation treatment at a high temperature of 200 to 400 ° C. in the presence of a noble metal-containing catalyst to perform purification. The processing method is usually 200 to 40
The reaction is usually carried out at a temperature of 0 ° C. in the presence of a noble metal catalyst by introducing hydrogen. The noble metal source is selected from palladium, ruthenium, rhodium, osmium, iridium, platinum and the like or a metal oxide thereof. These metals or metal oxides can be used as they are as catalysts, but those supported on a carrier such as activated carbon are particularly effective. The above contact treatment can be applied to either the continuous method or the batch method, but is particularly suitable for the continuous method.
The filter of the present invention is suitable as a filter for filtering the aqueous terephthalic acid solution after the treatment.

【0011】[0011]

【実施例】次に本発明について実施例および比較例をあ
げて、更に具体的に説明するが、本発明はその要旨を超
えない限り、以下の実施例に限定されるものではない。
Next, the present invention will be described more specifically with reference to examples and comparative examples. However, the present invention is not limited to the following examples unless it exceeds the gist thereof.

【0012】実施例1 パラキシレンを酢酸溶媒中で液相酸化して得られた粗テ
レフタル酸を250℃で純水に溶解し、30重量%のテ
レフタル酸水溶液とした。該水溶液を更に加熱し、粒状
活性炭に0.5%のパラジウムを担持させた触媒を充填
した反応塔に、温度290℃、圧力80kg/cm2
条件下、5重量部/hrで通液するとともに、反応塔入
口部より1.2容量部/hrの水素を供給した。反応塔
から流出してくるテレフタル酸水溶液を下記フィルター
に通過させて固形異物の除去を行った。フィルターの圧
損を測定したところ、連続運転を開始して6ケ月経過後
に初期値の約2倍となったので運転を中止した。6ケ月
の連続運転中、5〜10μmの固形異物の除去率は95
%であった。なお、異物の除去率は粒度分布計により測
定した。
Example 1 Crude terephthalic acid obtained by subjecting para-xylene to liquid phase oxidation in an acetic acid solvent was dissolved in pure water at 250 ° C. to obtain a 30% by weight terephthalic acid aqueous solution. The aqueous solution is further heated and passed through a reaction column filled with a catalyst having 0.5% palladium supported on granular activated carbon at a temperature of 290 ° C. and a pressure of 80 kg / cm 2 at 5 parts by weight / hr. At the same time, 1.2 parts by volume / hr of hydrogen was supplied from the inlet of the reaction tower. The terephthalic acid aqueous solution flowing out of the reaction tower was passed through the following filter to remove solid foreign substances. When the pressure loss of the filter was measured, the continuous operation was started, and after 6 months had elapsed, the operation was stopped because it became about twice the initial value. During the continuous operation for 6 months, the removal rate of solid foreign matter of 5 to 10 μm is 95
%Met. The foreign matter removal rate was measured by a particle size distribution meter.

【0013】(フィルターの構造) 穿孔されたボビン:内径25mm、外径30mm フランジ:外径80mm、フランジ間の間隔1000m
m カーボンファイバー巻線:糸径8μm、長さ10〜15
mmのカーボンファイバーのマルチフィラメント(集束
数約500本)を紬いで糸状とした紬糸を3本で撚り合
わせることにより得た太糸(糸径3.2mm)を綾角1
5°で厚さ15mmに巻回。
(Structure of Filter) Perforated bobbin: inner diameter 25 mm, outer diameter 30 mm Flange: outer diameter 80 mm, spacing between flanges 1000 m
m Carbon fiber winding: yarn diameter 8 μm, length 10 to 15
mm thick carbon fiber multifilaments (about 500 bundles) are threaded into three thread-like pongee yarns, and a thick yarn (yarn diameter 3.2 mm) obtained by twisting three yarns
Wound to a thickness of 15mm at 5 °.

【0014】比較例1 実施例1で用いたフィルターを下記フィルターに代えた
以外は実施例1と同様に実施したところ、連続運転50
日で圧損が初期値の約2倍となったので運転を中止し
た。また、この間の5〜10μmの固形異物の除去率は
75%であった。
Comparative Example 1 The same operation as in Example 1 was performed except that the filter used in Example 1 was changed to the following filter.
The operation was stopped because the pressure loss became about twice the initial value every day. During this period, the removal rate of 5 to 10 μm solid foreign matter was 75%.

【0015】(フィルターの構造)フィラメント単糸径
8μmのカーボンファイバーを用いて作成した不織布
(嵩密度0.06g/cm3 、厚さ10mm)とカーボ
ンクロス(10メッシュ、厚さ1mm)を交互に6段積
み重ねて厚さ15mmに圧縮し所定寸法に切断した後、
これを実施例1で用いたフランジ間の穿孔されたボビン
に巻きつけて作成した。
(Structure of Filter) A non-woven fabric (bulk density: 0.06 g / cm 3 , thickness: 10 mm) made of carbon fiber having a single filament diameter of 8 μm and carbon cloth (10 mesh, thickness: 1 mm) are alternately formed. After stacking 6 stages, compressing to a thickness of 15 mm, and cutting to predetermined dimensions,
This was wound around a bobbin perforated between the flanges used in Example 1 to make it.

【0016】[0016]

【発明の効果】本発明のフィルターによれば、高温、高
腐食性の溶液中の微細な固形異物を効率的に、かつ長期
間に亘り安定に除去することができる。工業的には、塩
酸、硫酸、硝酸等の無機強酸類や酢酸、テレフタル酸等
の有機酸類の製造工程で生ずる酸溶液の処理に好適であ
る。
According to the filter of the present invention, fine solid foreign matter in a high-temperature, highly corrosive solution can be efficiently and stably removed over a long period of time. Industrially, it is suitable for treating an acid solution generated in a process of producing inorganic strong acids such as hydrochloric acid, sulfuric acid and nitric acid, and organic acids such as acetic acid and terephthalic acid.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明のフィルターの1例を示す全体斜視図で
ある。
FIG. 1 is an overall perspective view showing one example of a filter of the present invention.

【図2】図1におけるフィルターの断面図である。FIG. 2 is a cross-sectional view of the filter in FIG.

【符号の説明】[Explanation of symbols]

1 :ボビン 2 :フランジ 3 :巻線 4 :空胴 5 :穿孔 1: bobbin 2: flange 3: winding 4: cavity 5: drilling

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 FI 技術表示箇所 C07C 63/26 2115−4H C07C 63/26 L (56)参考文献 特開 昭56−28615(JP,A) 特開 平2−171234(JP,A) 実開 平2−57123(JP,U) 実開 平1−170417(JP,U) 実開 平5−4013(JP,U) 実公 昭63−23940(JP,Y2)──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 6 Identification number Agency reference number FI Technical indication location C07C 63/26 2115-4H C07C 63/26 L (56) References JP-A-56-28615 (JP) JP-A-2-171234 (JP, A) JP-A-2-57123 (JP, U) JP-A-1-170417 (JP, U) JP-A-5-4013 (JP, U) 63-23940 (JP, Y2)

Claims (7)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 少なくとも一端が開放された孔を有する
ボビンの側面をカーボンファイバー・マルチフィラメン
トの撚糸で巻回被覆してなるフィルター。
1. A filter comprising a bobbin having at least one open end and a side surface wound with a carbon fiber multifilament twisted yarn.
【請求項2】 撚糸が、単糸径1〜20μm、長さ1〜
100mmのカーボンファイバーを紬いで糸状としたマ
ルチフィラメントを撚り合わせたものであることを特徴
とする請求項1のフィルター。
2. The twisted yarn has a single yarn diameter of 1 to 20 μm and a length of 1 to 20 μm.
2. The filter according to claim 1, wherein the multifilament is formed by twisting 100 mm carbon fiber into a thread shape.
【請求項3】 撚糸が、単糸径1〜20μmの連続糸を
集束し、ねじりを加えたマルチフィラメントを撚り合わ
せたものであることを特徴とする請求項1のフィルタ
ー。
3. The filter according to claim 1, wherein the twisted yarn is obtained by bundling continuous yarns having a single yarn diameter of 1 to 20 μm, and twisting multifilaments obtained by twisting.
【請求項4】 撚糸の糸径が2〜10mmであることを
特徴とする請求項2又は3のフィルター。
4. The filter according to claim 2, wherein the diameter of the twisted yarn is 2 to 10 mm.
【請求項5】 巻き厚が0.5〜5cmであることを特
徴とする請求項1ないし4のいずれかに記載のフィルタ
ー。
5. The filter according to claim 1, wherein the thickness of the filter is 0.5 to 5 cm.
【請求項6】 少なくとも一端が開放された複数個の孔
を有するボビンに該孔の全体を含み、所定間隔をあけて
2枚のフランジが設置され、該フランジ間においてボビ
ンの側面をカーボンファイバー・マルチフィラメントの
撚糸で巻回被覆してなる請求項1ないし5のいずれかに
記載のフィルター。
6. A bobbin having a plurality of holes at least one end of which is open, two flanges are provided at a predetermined interval, including the entirety of the holes, and a side of the bobbin is provided between the flanges by a carbon fiber. The filter according to any one of claims 1 to 5, which is wound and covered with a multifilament twisted yarn.
【請求項7】 撚糸を巻回する際の綾角が10〜20°
であることを特徴とする請求項1ないし6のいずれかに
記載のフィルター。
7. The winding angle of the twisted yarn is 10 to 20 °.
The filter according to any one of claims 1 to 6, wherein
JP7000694A 1995-01-06 1995-01-06 filter Expired - Lifetime JP2713198B2 (en)

Priority Applications (1)

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JP7000694A JP2713198B2 (en) 1995-01-06 1995-01-06 filter

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Application Number Priority Date Filing Date Title
JP7000694A JP2713198B2 (en) 1995-01-06 1995-01-06 filter

Related Parent Applications (1)

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JP3275734A Division JP2582970B2 (en) 1991-10-23 1991-10-23 Method for removing solid foreign matter from terephthalic acid aqueous solution

Publications (2)

Publication Number Publication Date
JPH07284618A JPH07284618A (en) 1995-10-31
JP2713198B2 true JP2713198B2 (en) 1998-02-16

Family

ID=11480878

Family Applications (1)

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Country Link
JP (1) JP2713198B2 (en)

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* Cited by examiner, † Cited by third party
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JP4256388B2 (en) * 2003-04-01 2009-04-22 日鉱金属株式会社 Tantalum sputtering target
JP2009034646A (en) * 2007-08-03 2009-02-19 Kurita Water Ind Ltd Pincushion filter and water treatment method
CN105384223A (en) * 2014-09-09 2016-03-09 浙江久新空气净化科技有限公司 Filter cloth capable of forming micro-electrolysis and application of filter cloth
CN114288720B (en) * 2021-12-31 2023-01-03 武汉大学 Carbon fiber filter, regeneration method thereof and carbon fiber filter device
CN114314957B (en) * 2021-12-31 2023-11-24 武汉大学 Electrode for electric flocculation-fiber filtering water treatment device, electric flocculation-fiber filtering water treatment device and use method thereof

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4278551A (en) * 1979-07-30 1981-07-14 Amf Incorporated Wound cartridge filters
JPS6323940U (en) * 1986-07-28 1988-02-17
JPH0612809Y2 (en) * 1988-05-23 1994-04-06 東洋濾紙株式会社 Nonwoven Wound Laminated Cartridge Filter with Net
JPH0719540Y2 (en) * 1988-10-13 1995-05-10 三菱レイヨン株式会社 Filter cylinder
JP2645118B2 (en) * 1988-12-23 1997-08-25 大阪瓦斯株式会社 Manufacturing method of laminate
JPH054013A (en) * 1991-04-26 1993-01-14 Toyota Autom Loom Works Ltd Cylindrical filter

Also Published As

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