JPS5927851A - Preparation of flake of terephthaloyl dichloride and/or isophthaloyl dichloride - Google Patents

Preparation of flake of terephthaloyl dichloride and/or isophthaloyl dichloride

Info

Publication number
JPS5927851A
JPS5927851A JP13665682A JP13665682A JPS5927851A JP S5927851 A JPS5927851 A JP S5927851A JP 13665682 A JP13665682 A JP 13665682A JP 13665682 A JP13665682 A JP 13665682A JP S5927851 A JPS5927851 A JP S5927851A
Authority
JP
Japan
Prior art keywords
resin
dichloride
synthetic resin
liquid
lined
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.)
Pending
Application number
JP13665682A
Other languages
Japanese (ja)
Inventor
Shinji Mita
真司 三田
Hiroshi Masai
宏 正井
Yuichi Yoshimura
祐一 吉村
Rokuro Inoue
井上 六郎
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 Gas Chemical Co Inc
Original Assignee
Mitsubishi Gas Chemical Co Inc
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
Application filed by Mitsubishi Gas Chemical Co Inc filed Critical Mitsubishi Gas Chemical Co Inc
Priority to JP13665682A priority Critical patent/JPS5927851A/en
Publication of JPS5927851A publication Critical patent/JPS5927851A/en
Pending legal-status Critical Current

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  • Glanulating (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

PURPOSE:To obtain colorless, high-quality flakes of the titled compound useful as a raw material of agricultural chemicals, pharmaceuticals, etc., by flaking terephthaloyl dichloride, etc. using a metallic drum etc. wherein the surface contacting with the liquid is lined with a synthetic resin. CONSTITUTION:Molten liquid of terephthaloyl dichloride and/or isophthaloyl dichloride heated preferably at a temperature higher than the melting point by 10-20 deg.C, is supplied to a metallic drum or steel bed lined with a synthetic resin or ceramic material at the surface of the part contacting with the liquid, and flaked under N2 gas stream. The synthetic resin is e.g. a fluorine resin such as polytrifluorochloroethylene, etc., a phenolic resin, a chlorinated polyether resin, a furan resin, etc., and the ceramic is, e.g. glass, alumina, zirconia, chromium oxide, etc. The thickness of the lining is 0.1-1.0mm., preferably 0.1-0.5mm.. USE:Raw material of engineering plastics, heat-resistant, high-modulus fibers, etc.

Description

【発明の詳細な説明】 本発明はテレフタル酸ジクロライド(以下、TPCと略
す)および/またはイソフタル酸ジクロライド(以下、
IPCと略す)のフレーク化法に関する。
Detailed Description of the Invention The present invention provides terephthalic acid dichloride (hereinafter abbreviated as TPC) and/or isophthalic acid dichloride (hereinafter abbreviated as TPC).
This invention relates to a flaking method for IPC (abbreviated as IPC).

TPC及びIPCは、エンジニアリングプラスチックス
、耐熱高弾性繊維、農薬、医薬などの原料として使用さ
れる化合物である。ところでTPC及びIPCは融点が
それぞれ約82℃及び約44℃であり、一般には常温で
固体である。そこで使用に際しては溶融されるが、TP
O及びIPCは溶融状態では昇華性を有すると共に、強
い刺激臭があり、特に工業的に大月に取り扱う上におい
て種々の回置な問題が伴う。
TPC and IPC are compounds used as raw materials for engineering plastics, heat-resistant high-elastic fibers, agricultural chemicals, medicines, and the like. By the way, TPC and IPC have melting points of about 82° C. and about 44° C., respectively, and are generally solid at room temperature. Therefore, when used, it is melted, but TP
In the molten state, O and IPC have sublimation properties and a strong pungent odor, and are accompanied by various problems, especially when handled industrially.

したがって、TPO及びIPCの製品の形態としては小
さく固形化することが望ましい。小さく固形化する方法
として従来より一般に知られている技術は、たとえば、
フレーク化する方法、大き1.c塊状の固形物を砕く方
法あるいは微粒状に造粒化する方法などがある。
Therefore, it is desirable that TPO and IPC products be made into small and solid forms. Conventionally known techniques for solidifying into small pieces include, for example,
How to make it into flakes: 1. c) There are methods such as crushing a lumpy solid material or granulating it into fine particles.

フレーク化する方法は、フレーカ−あるいはスチールベ
ルト等により、溶融状態の物質をフレーカ−ドラム表面
あるいはスチールベルト上KMい膜状にイ」着させ、こ
れを冷却、固化し、スクレーバーで該同化物をかき取る
周知の方法により得られる。
The method of flaking is to deposit a molten substance on the flaker drum surface or steel belt in the form of a thick film using a flaker or steel belt, cool and solidify it, and remove the assimilate using a scraper. Obtained by the well-known method of scraping.

T I) Cおよび/またはIPCをフレーク化するに
際して、従来市販のフレーク化装置を用いた場合には得
られるフレークはA P HA法により測定した場合の
色度が市<、エンジニアリングプラスチックス、*i用
の原料として用いることができなくなるなど、商品両値
が著しく低十する欠点がある。
T I) When forming C and/or IPC into flakes using a conventional commercially available flaking device, the resulting flakes have a chromaticity as measured by the APHA method. There are drawbacks such as the fact that it cannot be used as a raw material for i-products, and the value of both products is extremely low.

本発明者らは、上記の事情に鑑み、着色のな(・フレー
クを得るべく鋭意枚重した紀果、フレーカ−又i*−ス
チールベルトの接液部を合成樹脂又警]セラミックでラ
イニングすることにより着色が認められない良好なフレ
ークが得られることが認められた。
In view of the above circumstances, the inventors of the present invention have developed a method to line the wetted parts of a steel belt with synthetic resin and ceramic, without coloring. It was found that good flakes with no coloration were obtained.

すなわち、本発明は、テレフタル酸ジクロライドおよび
/またはイソフタル酸ジクロライドをフレーク化するに
際し、合成樹脂またをまセラミックで接液部の表面がラ
イニングされた金属製ドラムあるい(まスチールベルト
を用いることを特徴とするフレーク化法に関する。
That is, the present invention uses a metal drum (or steel belt) whose surface in contact with liquid is lined with synthetic resin or ceramic when turning terephthalic acid dichloride and/or isophthalic acid dichloride into flakes. Regarding the characteristic flaking method.

本発明において、ライニングに用いられる合成樹脂とし
てはフッ素化樹脂、フェノール樹脂、塩素化ポリエーテ
ル樹脂、フラン樹脂等ケあげることができる。
In the present invention, the synthetic resins used for the lining include fluorinated resins, phenol resins, chlorinated polyether resins, furan resins, and the like.

フッ素化樹脂としては、例えば、ポリ三フッ化塩化エチ
レン、ポリ四フッ化エチレン、四フッ化エチレンー六フ
ッ化プロピレン共重合物、四フッ化エチレンーエチレン
共重合物、四フフ化エチレンーバーフルオロアルコキシ
ェヂレン共重合物、ポリフッ化ビニリデン等の炭素鎖に
フッ素が結合した樹脂゛をあげることができる。
Examples of fluorinated resins include polytrifluorochloroethylene, polytetrafluoroethylene, tetrafluoroethylene-hexafluoropropylene copolymer, tetrafluoroethylene-ethylene copolymer, and tetrafluoroethylene-perfluoroethylene. Examples include resins in which fluorine is bonded to the carbon chain, such as alkoxyshedylene copolymers and polyvinylidene fluoride.

フェノール樹脂としては、フェノール樹脂およびフェノ
ール樹脂を主成分としたブレンド物をあげることができ
る。
Examples of the phenolic resin include phenolic resins and blends containing phenolic resins as main components.

また、ライニングK JTiいられるセラミックとして
は、カラス、アルミナ、ジルコニア、酸化クロムなどを
あげることができる。
Furthermore, examples of ceramics that can be used as the lining KJTi include glass, alumina, zirconia, and chromium oxide.

フレーク化に際しては、溶融液より速やかに除熱する必
要があることがらライニング材の熱伝導性はできるだけ
大きい方が好ましい。本発明に用いられる合成樹脂ある
(・はセラミックは熱伝導性が鉄に比べ小さく、熱伝導
度は一般に鉄の1/20〜11500である。したがっ
て、ライニングの膜厚はできるだけ薄い方が好ましい。
When flaking, it is necessary to remove heat more quickly than from the molten liquid, so it is preferable that the thermal conductivity of the lining material be as high as possible. The thermal conductivity of the synthetic resin ceramic used in the present invention is lower than that of iron, and the thermal conductivity is generally 1/20 to 11,500 that of iron. Therefore, it is preferable that the thickness of the lining be as thin as possible.

しかし余りにも薄過ぎると作業中にライニングの膜が剥
離する危険性がある。これらの点を考虜し、膜厚は0.
1〜1.0別層度、好ましくけ0.1〜0.5mInで
ある。
However, if it is too thin, there is a risk that the lining film will peel off during work. Considering these points, the film thickness was set to 0.
The layer thickness is 1 to 1.0 mIn, preferably 0.1 to 0.5 mIn.

フレーク化にあたり、供給される’I’ P C又は1
− P Cの溶融液の温度は融点より30℃程度高め、
好ましくは融点より10〜20℃高めが良い。また、冷
却面の温度は理論的には融点以下の温度であれば良いが
、好ましくは融点より30℃以下にするのが好ましい。
'I' P C or 1 supplied for flaking
- The temperature of the PC melt is about 30℃ higher than the melting point,
Preferably, the temperature is 10 to 20°C higher than the melting point. The temperature of the cooling surface should theoretically be below the melting point, but it is preferably 30° C. below the melting point.

さら[、TPC及びI PC,またはこれらの混合物は
水と反応して容易に加水分解するので、フレーク化に聞
しては、装置内は窒累気流−ト、あるいは乾燥望気気流
下にし、装置外の湿気を6Xびた大気との接触を断つこ
とが必要である。
Furthermore, since TPC, IPC, or a mixture thereof reacts with water and is easily hydrolyzed, for flaking, the inside of the apparatus should be placed under a nitrogen stream or a dry air stream. It is necessary to cut off contact with the 6X moist atmosphere outside the device.

以上、本発明σ)方法によれば着色のなし・商品ησ)
フレーク状TPC及び/又はIPCを得ることができ、
本発明f’l−工業的に極めて意義の高いものである。
As mentioned above, according to the method of the present invention σ), no coloring/product ησ)
flaky TPC and/or IPC can be obtained,
The present invention f'l is of extremely high industrial significance.

以−干に実施例を記す。Examples are described below.

実施例 95℃f加熱時の色度1o (APHA法)の1”Pc
(純度 99,91%)をガラスライニング製σ)容器
に入れ、内面が40″CIC冷却された、1分間に2.
5回回転するポリ三フッ化塩化エチレンでライニングさ
れたフレーカ−ドラムと接触させた。ドラムの周りに固
化したTPOを塩化ビニル製スクレーバーでかき取りフ
レーク状のTPCを得た。フレーク化された1゛PCの
色度(APHA法)及び純度は原料のTPOのそれらと
同じであった。
Example 9 1"Pc of chromaticity 1o (APHA method) when heated at 5℃f
(purity 99.91%) was placed in a glass-lined σ) container, and the inner surface was cooled by 40"CIC.
Contact was made with a polytrifluorochloroethylene lined flaker drum which was rotated five times. The solidified TPO around the drum was scraped off with a vinyl chloride scraper to obtain flaky TPC. The chromaticity (APHA method) and purity of the flaked 1'PC were the same as those of the raw TPO.

比較の目的で、ライニングされていない市販の通常の鉄
製のフレーカ−ドラムを用いてフレーク状のTPCを得
た。(↓iられたフレーク状TP Cの純度は上記実施
例と変わりがなかったが、色度(APHA法)が40で
おうた。
For comparison purposes, TPC flakes were obtained using a commercially available conventional iron flaker drum without lining. (↓The purity of the obtained flaky TPC was the same as in the above example, but the chromaticity (APHA method) was set at 40.

特許出願人  三菱瓦斯化学株式会社 代表者長野和吉Patent applicant: Mitsubishi Gas Chemical Co., Ltd. Representative Kazuyoshi Nagano

Claims (1)

【特許請求の範囲】 1)テレフタル酸ジクロライドおよび/またGマイソフ
タル酸ジクロライドをフレーク化するに際し、合成樹脂
またはセラミックで接液部の表面がライニングされた金
属製ドラムある(・目スチールベルトを用いることを特
徴とするフレーク化法。 2)」二記合成樹脂が、フッ素化樹脂、フェノール樹脂
、塩素化ポリエーテル樹脂、フラン樹脂から選ばれる一
種である特許請求の範囲第1項記載の方法 3)上記セラミックがガラス、アルミナ、ジルコニア、
酸化クロムから選ばれる一種である特許請求の範囲第1
項記載の方法。
[Claims] 1) When turning terephthalic acid dichloride and/or G-mysophthalic acid dichloride into flakes, there is a metal drum whose surface in contact with the liquid is lined with synthetic resin or ceramic (a steel belt is used). 2) The method according to claim 1, wherein the synthetic resin is one selected from fluorinated resins, phenol resins, chlorinated polyether resins, and furan resins. The above ceramics are glass, alumina, zirconia,
Claim 1 which is a type selected from chromium oxide
The method described in section.
JP13665682A 1982-08-05 1982-08-05 Preparation of flake of terephthaloyl dichloride and/or isophthaloyl dichloride Pending JPS5927851A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13665682A JPS5927851A (en) 1982-08-05 1982-08-05 Preparation of flake of terephthaloyl dichloride and/or isophthaloyl dichloride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13665682A JPS5927851A (en) 1982-08-05 1982-08-05 Preparation of flake of terephthaloyl dichloride and/or isophthaloyl dichloride

Publications (1)

Publication Number Publication Date
JPS5927851A true JPS5927851A (en) 1984-02-14

Family

ID=15180424

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13665682A Pending JPS5927851A (en) 1982-08-05 1982-08-05 Preparation of flake of terephthaloyl dichloride and/or isophthaloyl dichloride

Country Status (1)

Country Link
JP (1) JPS5927851A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2691377A1 (en) * 1992-05-21 1993-11-26 Inst Francais Du Petrole Rotary oven for chemical reaction.
FR2691378A1 (en) * 1992-05-21 1993-11-26 Inst Francais Du Petrole Sulphurisation process for catalysers - using a rotating tube coated with e.g. alumina to prevent occurrence of sec. reactions

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2691377A1 (en) * 1992-05-21 1993-11-26 Inst Francais Du Petrole Rotary oven for chemical reaction.
FR2691378A1 (en) * 1992-05-21 1993-11-26 Inst Francais Du Petrole Sulphurisation process for catalysers - using a rotating tube coated with e.g. alumina to prevent occurrence of sec. reactions

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