JPS6067532A - Cleaning of equipment attached with polyamide - Google Patents
Cleaning of equipment attached with polyamideInfo
- Publication number
- JPS6067532A JPS6067532A JP17639483A JP17639483A JPS6067532A JP S6067532 A JPS6067532 A JP S6067532A JP 17639483 A JP17639483 A JP 17639483A JP 17639483 A JP17639483 A JP 17639483A JP S6067532 A JPS6067532 A JP S6067532A
- Authority
- JP
- Japan
- Prior art keywords
- cleaning
- polyamide
- equipment
- washing
- 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.)
- Granted
Links
Landscapes
- Polyamides (AREA)
- Moulds For Moulding Plastics Or The Like (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、ポリアミドの付着によって汚れた装置類を再
度使用するために、付着しているポリアミドを洗浄除去
する方法に関するものであり、さらに詳しくは、ポリア
ミドの付着した装置類に多価アルコール類と、ジカルボ
ン酸および/またはジカルボン酸無水物とから主として
なる洗浄液を180℃以上の温度で接触させることによ
り、洗浄力が高く、装置への悪影響がなく、シかも使用
後の洗浄液の処理が容易である洗浄方法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for cleaning and removing equipment contaminated with polyamide in order to use the equipment again. By contacting a cleaning liquid mainly consisting of polyhydric alcohols and dicarboxylic acid and/or dicarboxylic acid anhydride at a temperature of 180°C or higher, the cleaning power is high, there is no adverse effect on the equipment, and it is easy to clean after use. The present invention relates to a cleaning method in which cleaning liquid can be easily processed.
ポリアミド繊維等を製造する場合に使用される製造装置
、例えば重合装置、成形装置、紡糸装置、それらの付属
装置は、使用する過程でポリアミドが付着して汚れる。Manufacturing equipment used in manufacturing polyamide fibers, such as polymerization equipment, molding equipment, spinning equipment, and their auxiliary equipment, becomes contaminated with polyamide during use.
この付着したポリアミドは、ポリアミドの種類あるいは
ポリアミド組成物の品種を変更する場合、洗浄除去する
ことが必要である。また、付着したポリアミドが長期間
の運転で変性して、異物となって、製品ポリアミドを汚
染することもあり、この場合も洗浄が必要である。This adhered polyamide must be removed by washing when changing the type of polyamide or the type of polyamide composition. Further, the adhered polyamide may denature during long-term operation and become foreign matter that contaminates the product polyamide, and cleaning is also required in this case.
従来、ポリアミド製造装置に付着しているポリアミドを
洗浄除去するには、アルカリ金属類の硝酸塩等を高温で
溶解させた液中に、装置を浸漬して洗浄する方法、高温
のサンドに接触させて洗浄する方法、または高温の希リ
ン酸溶液に接触させる方法等が採用されていた。これら
の方法は、複雑かつ精密化しているポリアミド製造装置
類を変形させたり、腐食させたりする欠点があり、さら
に可燃性ガスが発生してアフター処理が必要になり、安
全上も問題があった。Conventionally, in order to wash and remove polyamide adhering to polyamide production equipment, there have been two methods: cleaning the equipment by immersing it in a liquid in which nitrates of alkali metals, etc. are dissolved at high temperature, and cleaning the equipment by exposing it to hot sand. Methods such as washing or contacting with a high temperature dilute phosphoric acid solution have been adopted. These methods have the drawback of deforming or corroding the complex and sophisticated polyamide manufacturing equipment, and also generate flammable gas, requiring after-treatment, which poses safety issues. .
また、有機溶媒単独の洗浄液やこれに添加剤を併用した
洗浄液も種々提案されてきているが、洗浄剤としてはま
だ不十分であったり、あるいけ洗浄力は満足するが、添
加剤の中和が必要であったりする欠点があり、実用上問
題があった。In addition, various cleaning solutions using organic solvents alone and additives have been proposed, but some of them are still insufficient as cleaning agents, and some have satisfactory cleaning power but do not neutralize the additives. This method has the disadvantage that it sometimes requires the use of a conventional method, which poses a practical problem.
例えば、ドイツ特許第1188212号および同第11
48875号の明細書では、−価あるいは多価アルコー
ルを洗浄剤とする方法が提案されている。この方法は、
常圧の場合、ポリアミドを溶解する能力が低く、十分に
洗浄するためには長時間を要するし、また、沸点以上の
加圧にしても常圧より時間は短くなるが、洗浄力はまだ
十分でないという欠点があった。また、特公昭51−4
7477号公報では、多価アルコール類にアルカリ金属
またはアルカリ土類金属の化合物もしくは、鉱酸を添加
した組成物を洗浄剤とする方法を提案しているが、この
方法は使用後の洗浄液全廃棄する際に、酸あるいはアル
カリで中和しなければならないし、また、鉱酸使用の場
合は、装置材質の腐食を生じ、一方、アルカリ金属、ア
ルカリ土類金属化合物使用の場合は装置材質の腐食割れ
を生じるおそれがあるという欠点があった。For example, German Patent No. 1188212 and German Patent No. 11
The specification of No. 48875 proposes a method using -hydric or polyhydric alcohol as a cleaning agent. This method is
In the case of normal pressure, the ability to dissolve polyamide is low and it takes a long time to thoroughly clean it.Also, even if pressure is applied above the boiling point, the time will be shorter than normal pressure, but the cleaning power is still sufficient. There was a drawback that it was not. In addition, special public service 51-4
Publication No. 7477 proposes a method of using a composition in which an alkali metal or alkaline earth metal compound or a mineral acid is added to a polyhydric alcohol as a cleaning agent, but this method requires the entire cleaning solution to be disposed of after use. When cleaning, it must be neutralized with acid or alkali, and if mineral acids are used, equipment materials will corrode, whereas if alkali metals or alkaline earth metal compounds are used, equipment materials will corrode. There was a drawback that there was a risk of cracking.
本発明者らは、洗浄能力が十分に高く、しかも洗浄廃液
全廃棄する場合中和を必要とせず、装置材質に対し腐食
のおそれがない洗浄液について鋭意検討した結果、本発
明をなすに至ったのである。The present inventors have made the present invention as a result of extensive research into a cleaning solution that has a sufficiently high cleaning ability, does not require neutralization when all cleaning waste liquid is disposed of, and does not cause corrosion to equipment materials. It is.
すなわち、本発明は、多価アルコール類と、ジカルボン
酸およびジカルボン酸無水物の群から選ばれた1種以上
の化合物(以下、ジカルボン酸類という)とから主とし
てなる洗浄液を、180℃以上の温度で、ポリアミドの
付着した装置類と接触させることにより、前記ポリアミ
ドを装置類から分離除去させる洗浄方法からなるもので
あって、装置類の変形、損傷、腐食がなく、洗浄液もp
Hが中性もしくは中性に近いので洗浄廃液の処理が容易
であるという優れた特徴を有するものである。That is, the present invention provides a method of cleaning a cleaning liquid mainly consisting of a polyhydric alcohol and one or more compounds selected from the group of dicarboxylic acids and dicarboxylic anhydrides (hereinafter referred to as dicarboxylic acids) at a temperature of 180°C or higher. , a cleaning method in which the polyamide is separated and removed from the equipment by bringing it into contact with the equipment to which polyamide has adhered, and the equipment is not deformed, damaged, or corroded, and the cleaning solution is also free of P.
Since H is neutral or close to neutral, it has the excellent feature that washing waste liquid can be easily treated.
本発明で使用する洗浄液の溶媒としては、ジカルボン酸
類を添加して使用できる点から多価アルコール類が用い
られる。該多価ア/lz :l−ル類として使用できる
化合物としては、メチレングリコール系、エチレングリ
コール系、プロピレングリコール系、グリセリンなどの
ジオール、トリオールなどがあげられるが、特に好まし
いのはエチレングリコール、ジエチレンクリコール、ト
リエチレングリコールである。As the solvent for the cleaning liquid used in the present invention, polyhydric alcohols are used since they can be used with addition of dicarboxylic acids. Compounds that can be used as the polyhydric alcohols include diols and triols such as methylene glycol, ethylene glycol, propylene glycol, and glycerin, but particularly preferred are ethylene glycol and diethylene. Glycol, triethylene glycol.
また、ジカルボン酸類として使用できる化合物としては
、コへり酸、メチルコハク酸、グルタル酸、アジピン酸
、アゼライン酸、セバシン酸、シクロヘキサンジカルボ
ン酸、フタル酸、イソフタル酸、テレフタル酸、無゛水
コハク酸、無水メチルコハク酸、無水グルタル酸、無水
マレイン酸、無水フタル酸、これら化合物の主鎖内にア
ルキル基、脂環基、芳香族基、ヘテロ原子を置換基とし
て含む化合物等の如き、洗浄濡麿において分解しない、
脂肪族、脂環族、芳香族のジカルボン酸およびジカルボ
ン酸無水物があげられるが、なかでも脂肪族ジカルボン
酸とその無水物が好ましい。Compounds that can be used as dicarboxylic acids include succinic acid, methylsuccinic acid, glutaric acid, adipic acid, azelaic acid, sebacic acid, cyclohexanedicarboxylic acid, phthalic acid, isophthalic acid, terephthalic acid, succinic anhydride, and anhydrous Methylsuccinic acid, glutaric anhydride, maleic anhydride, phthalic anhydride, and compounds containing alkyl groups, alicyclic groups, aromatic groups, and heteroatoms as substituents in the main chain of these compounds, etc., are decomposed during washing and wet cleaning. do not,
Examples include aliphatic, alicyclic, and aromatic dicarboxylic acids and dicarboxylic anhydrides, with aliphatic dicarboxylic acids and their anhydrides being particularly preferred.
洗浄液として使用する多価アルコール類およびジカルボ
ン酸類の沸点が180℃未満であると、180℃以上で
行なう洗浄時に必ず加圧しなくてはならないという欠点
があるので、沸点180℃以上の化合物であることが好
ましい。また、同様に、洗浄を加圧せず常圧で行なうた
めには、洗浄時の温度以上の沸点を有する化合物を選択
することが好ましい。If the boiling point of the polyhydric alcohols and dicarboxylic acids used as the cleaning liquid is less than 180°C, there is a disadvantage that pressure must be applied when cleaning is carried out at 180°C or higher, so the compound must have a boiling point of 180°C or higher. is preferred. Similarly, in order to perform washing at normal pressure without pressurization, it is preferable to select a compound having a boiling point higher than the temperature during washing.
゛ −
ジカルボン酸類の添加量は、多価アルコール類に対して
0.5重量%〜20重量%であることが好ましく、特に
1重量%〜1o重量%が好適である。0.5重量%未満
では、ポリアミドの溶解に長時間を要し、ポリマーが装
置類に残留することがあるので好ましくない。また、2
0重量%を越えると常温時における洗浄液が粘稠あるい
はペースト状になって、取扱い作業性が悪くなったり、
洗浄後の装置類を水洗するのに時間を要するので好まし
くない。- The amount of dicarboxylic acids added is preferably 0.5% to 20% by weight, particularly preferably 1% to 10% by weight, based on the polyhydric alcohol. If it is less than 0.5% by weight, it will take a long time to dissolve the polyamide and the polymer may remain in equipment, which is not preferable. Also, 2
If it exceeds 0% by weight, the cleaning solution at room temperature becomes viscous or paste-like, resulting in poor handling and workability.
This is not preferable because it takes time to wash the equipment after washing.
本発明で用いる洗浄液は、前記多価アルコール類と前記
ジカルボン酸類とからなるもの、あるいはこれら洗浄液
を主としてなるものであり、上記二成分の他に洗浄効果
全阻害しない範囲で他の溶剤を併用してもよい。The cleaning liquid used in the present invention is composed of the polyhydric alcohols and the dicarboxylic acids, or is mainly composed of these, and in addition to the above two components, other solvents may be used in combination as long as the cleaning effect is not completely impaired. It's okay.
洗浄温度は、180℃以上で前記洗浄液にポリアミドの
付着した装置類を接触させればよい。The cleaning temperature may be 180° C. or higher, and the equipment to which polyamide is attached may be brought into contact with the cleaning liquid.
洗浄液を攪拌したり、ポンプで循環させなりまたは、不
活性ガスでバブリングさせることにより洗浄時間を速め
ることもできる。The cleaning time can also be accelerated by stirring the cleaning solution, circulating it with a pump, or bubbling it with an inert gas.
本発明で用いた洗浄液は、180℃以上で洗浄すれば加
圧しなくても十分良好な洗浄効果を奏するので、洗浄装
置の点から常圧下での洗浄が好ましいが、加圧下で行な
っても支障はない。The cleaning liquid used in the present invention exhibits a sufficiently good cleaning effect even without pressurization if it is cleaned at 180°C or higher, so cleaning under normal pressure is preferable from the viewpoint of cleaning equipment, but cleaning under pressure may cause problems. There isn't.
洗浄液の各成分の沸点以上の温度で洗浄する場合は、加
圧釜を使用して加圧下で行なうことが好ましいが、還流
装置を付けて常圧下で行なってもよい。When washing at a temperature higher than the boiling point of each component of the washing liquid, it is preferable to use a pressure cooker to carry out the washing under pressure, but it is also possible to use a reflux device and carry out the washing under normal pressure.
”! ft 、沸点以下で洗浄する場合でも洗浄液の蒸
散を防ぐために還流装置を付け、安全上問題とならない
処理をすることが望ましい。ft. Even when cleaning at temperatures below the boiling point, it is desirable to install a reflux device to prevent the cleaning liquid from evaporating, and to ensure that the process does not pose a safety problem.
洗浄時の温度が180℃未満では、ポリアミドを溶解さ
せるのに長時間を要したり、装置類にポリマーが残留し
たりしてポリアミド全洗浄除去する目的を十分に達する
ことができないので、180℃以上で洗浄する必要があ
る。If the cleaning temperature is less than 180°C, it will take a long time to dissolve the polyamide, and the polymer will remain in the equipment, making it impossible to fully remove the polyamide. It is necessary to wash with the above.
本発明法により、ポリアミド付着装置類を洗浄すると、
付着しているポリアミド(その変性物も含む)を十分に
洗浄除去することができ、しかも、洗浄時に、装置類の
腐食を生じるおそれがないので、紡糸口金、紡糸パック
、重合釜の如きポリアミド付着装置類の洗浄法として好
適であり、特に、装置類の腐食のおそれがない点から、
紡糸口金、紡糸パック内の口金部品の如き、精度が要求
される装置類の洗浄法として好適である。また、洗浄廃
液の廃棄時に中和する必要がないという優れた効果もあ
る。When polyamide deposition equipment is cleaned by the method of the present invention,
Adhering polyamide (including its modified products) can be sufficiently washed away, and there is no risk of corrosion of equipment during cleaning, so polyamide adhesion such as spinnerets, spinning packs, and polymerization kettles can be removed. It is suitable as a method for cleaning equipment, especially since there is no risk of corrosion of equipment.
This method is suitable for cleaning equipment that requires precision, such as spinnerets and spinneret parts in spinning packs. Another advantageous effect is that there is no need to neutralize cleaning waste liquid when disposing of it.
次に本発明を実施例をあげて具体的に説明する。Next, the present invention will be specifically explained by giving examples.
拳 実施例1
ナイロン6の紡糸に使用して、ポリアミドの付着した紡
糸口金を金属製バスケットに入れ、ジエチレングリコー
ル100重量部と、コハク酸5重量部とからなる洗浄液
全入れた槽中に、前記バスケットごと浸した。次いで水
冷式還流装置を付け、槽の底部から窒素ガスをバブリン
グさせながら加熱を始めた。Fist Example 1 A spinneret used for spinning nylon 6 and coated with polyamide was placed in a metal basket, and the basket was placed in a tank containing a cleaning solution consisting of 100 parts by weight of diethylene glycol and 5 parts by weight of succinic acid. I soaked it all in. Next, a water-cooled reflux device was attached, and heating was started while bubbling nitrogen gas from the bottom of the tank.
240℃で8時間保った後、洗浄液を抜き、バスケット
を自然冷却後、紡糸口金を取り出し、次いで水洗、超音
波洗浄、水洗を2回くり返して行ない、口金全エアブロ
−して乾かした。After being kept at 240° C. for 8 hours, the cleaning solution was drained, and the basket was naturally cooled, and then the spinneret was taken out, followed by water washing, ultrasonic washing, and water washing twice, and the spinneret was completely dried by air blowing.
この紡糸口金を、顕微鏡観察したところ、口金孔内には
ナイロン6ポリマーの付着は全くみられなかった。When this spinneret was observed under a microscope, no nylon 6 polymer was observed inside the spinneret holes.
この洗浄液は引き続き、ナイロン6ポリマーの付着した
紡糸口金、ポーラスメタルおよびフィルター等の口金部
品の洗浄に繰返し5回使用したが、洗浄後の紡糸口金や
口金部品には、付着物は全く残っていなかった。This cleaning solution was subsequently used five times to clean spinnerets, porous metals, filters, and other spinnerets to which nylon 6 polymer had adhered, but no deposits remained on the spinnerets or spinneret parts after cleaning. Ta.
5回使用後の洗浄液50−を取り、250 mlまで水
で希釈した液のpHは4.7であり、1回使用後の洗浄
液ではp H4,2であったので、中和せずに廃棄する
ことができた。The pH of the 50-mL solution taken after 5 uses and diluted with water to 250 ml was 4.7, and the pH of the solution after 1 use was 4.2, so it was discarded without neutralization. We were able to.
・ 実施例2
ナイロン66の重合を終了してポリマーを排出した後、
内壁にポリアミドの付着している容量1001の重合釜
に、トリエチレングリコール100重量部とアジピン酸
4重量部とからなる洗浄液751を仕込み、密閉にして
から加熱・攪拌全開始した。260℃で2時間保ち、そ
の後冷却を開始し100℃に達した時重合釜の底から洗
浄液を抜き取った。あらかじめ95℃に予熱した水を重
合釜に満たして、20分間攪拌後、′水を排出し、さら
に常温水で2回洗浄を繰返した。水洗浄を終った重合釜
を解体して、内壁および攪拌俸を検査した結果)ポリマ
ーの付着は全くなかった。使用後の洗浄液を水で5倍量
うすめた液のpHは4.5であったので、中和せずに廃
棄することができた。- Example 2 After finishing the polymerization of nylon 66 and discharging the polymer,
A cleaning solution 751 consisting of 100 parts by weight of triethylene glycol and 4 parts by weight of adipic acid was charged into a polymerization kettle having a capacity of 1001 and having polyamide attached to the inner wall, and after the vessel was sealed, heating and stirring were started. The temperature was kept at 260°C for 2 hours, and then cooling was started, and when the temperature reached 100°C, the washing liquid was drawn out from the bottom of the polymerization vessel. The polymerization pot was filled with water preheated to 95° C., and after stirring for 20 minutes, the water was discharged and washing was repeated twice with room temperature water. The polymerization pot was dismantled after washing with water, and the inner wall and stirring barrel were inspected. As a result, there was no polymer adhesion at all. The pH of the used cleaning solution diluted five times with water was 4.5, so it could be disposed of without neutralization.
・ 実施例8〜10
SUS−804のステンレス鋼ピースに各種ポリアミド
を溶融付着させた試料片を用いて、第1表に示す組成か
らなる洗浄液を入れたガラスフラスコに、ガラス管制の
空冷還流器を付し、マントルヒーターで所定の温度と時
間、窒素ガスバブリングしながら加熱した。冷却後、試
料片を取り出し、水で水洗後、試料片を目視観察した。・Examples 8 to 10 Using a sample piece made of SUS-804 stainless steel piece to which various polyamides were melted and adhered, a glass flask containing a cleaning solution having the composition shown in Table 1 was placed in a glass-controlled air-cooled reflux device. The sample was then heated using a mantle heater at a predetermined temperature and time while bubbling nitrogen gas. After cooling, the sample piece was taken out, washed with water, and then visually observed.
その結果と使用後の洗浄液のpHを第1表に示した。The results and the pH of the cleaning solution after use are shown in Table 1.
洗浄液のpH測定法は、実施例1と同じである。The method for measuring the pH of the cleaning solution was the same as in Example 1.
なお、試料片の外観および色調は、加熱前に比べ変化は
認められなかった。Note that no change was observed in the appearance and color tone of the sample piece compared to before heating.
・ 比較例1〜5
洗浄液組成を第2表のとおり変えた以外は、実施例8〜
8と同様な方法で試料片全洗浄した。その結果を第2表
に示した。- Comparative Examples 1 to 5 Examples 8 to 5 except that the cleaning solution composition was changed as shown in Table 2.
The sample piece was completely washed in the same manner as in 8. The results are shown in Table 2.
比較例1・2は、ポリマーが残留付着していた。In Comparative Examples 1 and 2, residual polymer remained attached.
比較例3・4・5は、ポリマーの付着は全くなかったが
、洗浄液のpHが強アルカリ性もしくは強酸性を示した
ので、洗浄液を廃棄する際、中和しなくてはならなかっ
た。また、比較例5は洗浄液が黒色となり、試料片も、
一部黒色の斑点があり、明らかに腐食されていることが
認められた。In Comparative Examples 3, 4, and 5, there was no polymer adhesion at all, but the pH of the cleaning solution was strongly alkaline or acidic, so the cleaning solution had to be neutralized when discarded. In addition, in Comparative Example 5, the cleaning liquid turned black, and the sample piece also became black.
There were some black spots, and it was clearly observed that there was corrosion.
Claims (1)
無水物の群から選ばれた一種以上の、化合物とから主と
してなる洗浄液を、180℃以上の温度でポリアミドの
付着した装置類と接触させ、前記ポリアミドを洗浄除去
することを特徴とするポリアミドの付着した装置類の洗
浄方法。A cleaning solution mainly consisting of polyhydric alcohols and one or more compounds selected from the group of dicarboxylic acids and dicarboxylic acid anhydrides is brought into contact with equipment on which polyamide is attached at a temperature of 180° C. or higher to remove the polyamide. A method for cleaning equipment on which polyamide is attached, characterized by cleaning and removing it.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP17639483A JPS6067532A (en) | 1983-09-26 | 1983-09-26 | Cleaning of equipment attached with polyamide |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP17639483A JPS6067532A (en) | 1983-09-26 | 1983-09-26 | Cleaning of equipment attached with polyamide |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS6067532A true JPS6067532A (en) | 1985-04-17 |
JPS6365203B2 JPS6365203B2 (en) | 1988-12-15 |
Family
ID=16012890
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP17639483A Granted JPS6067532A (en) | 1983-09-26 | 1983-09-26 | Cleaning of equipment attached with polyamide |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS6067532A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006082253A (en) * | 2004-09-14 | 2006-03-30 | Toyota Motor Corp | Mold washing method |
-
1983
- 1983-09-26 JP JP17639483A patent/JPS6067532A/en active Granted
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006082253A (en) * | 2004-09-14 | 2006-03-30 | Toyota Motor Corp | Mold washing method |
Also Published As
Publication number | Publication date |
---|---|
JPS6365203B2 (en) | 1988-12-15 |
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