JPH0615492B2 - Purification method of acetic anhydride - Google Patents
Purification method of acetic anhydrideInfo
- Publication number
- JPH0615492B2 JPH0615492B2 JP8277486A JP8277486A JPH0615492B2 JP H0615492 B2 JPH0615492 B2 JP H0615492B2 JP 8277486 A JP8277486 A JP 8277486A JP 8277486 A JP8277486 A JP 8277486A JP H0615492 B2 JPH0615492 B2 JP H0615492B2
- Authority
- JP
- Japan
- Prior art keywords
- acetic anhydride
- diketene
- treatment
- purification method
- raw material
- 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
Links
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は無水酢酸の精製方法に関するものである。無水
酢酸は、アセチルセルロースの原料、医薬、農薬、染料
などに広く用いられている。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for purifying acetic anhydride. Acetic anhydride is widely used as a raw material for acetyl cellulose, medicines, agricultural chemicals, dyes and the like.
（従来技術および問題点） 無水酢酸の製法としては、酢酸、アセトンまたは酢酸メ
チル、酢酸エチル等の蒸気を熱分解して、生成するケテ
ンガスを酢酸に吸収、反応させて得る方法、無水塩化ア
ルミなどを触媒として酢酸にホスゲンと反応させる方
法、またはエチリデンジアセテートを塩化亜鉛等触媒の
存在下で加熱する方法などが知られている。これら公知
の方法で得られる無水酢酸には副反応として、ケテン自
身の２量化によるジケテンの生成、および反応工程等
で、無水酢酸自身の熱的経変等で生成すると考えられる
ジケテンが無水酢酸中に混入し、これらの無水酢酸を、
蒸留等公知の方法で精製しようとした場合、無水酢酸と
ジケテンとの沸点差が小さいこともあり、高還流比高段
数の精密蒸留を行う必要があり、エネルギーコストが高
いという問題があった。又、エネルギーコストを無視し
たとしても本発明のようにジケテンが不検出（5PPM以
下）の無水酢酢酸を得ることは不可能であった。(Prior art and problems) As a method for producing acetic anhydride, a method in which vapor such as acetic acid, acetone or methyl acetate, ethyl acetate is thermally decomposed to absorb and react the produced ketene gas with acetic acid, anhydrous aluminum chloride, etc. There is known a method of reacting acetic acid with phosgene by using as a catalyst or a method of heating ethylidene diacetate in the presence of a catalyst such as zinc chloride. As a side reaction, acetic anhydride obtained by these known methods produces diketene by dimerization of ketene itself, and diketene, which is considered to be generated by thermal aging of acetic anhydride itself in a reaction step or the like, in acetic anhydride. And mix these acetic anhydrides with
In the case of purifying by a known method such as distillation, the boiling point difference between acetic anhydride and diketene may be small, and it is necessary to carry out precision distillation with a high reflux ratio and a high number of stages, resulting in a high energy cost. Further, even if the energy cost was ignored, it was impossible to obtain acetic anhydride without diketene detection (5 PPM or less) as in the present invention.
ジケテンは非常に反応性が高いため、特に医薬、農薬、
洗顔料等の原料に使用する無水酢酸は、不純物としての
ジケテンの含有量によってその商品価値が著しく左右さ
れる。Diketene is very reactive, so
The commercial value of acetic anhydride used as a raw material for facial cleansers and the like significantly depends on the content of diketene as an impurity.
本発明は、工業的に有利にジケテン含有量の少い高品質
の無水酢酸を得るための精製方法を提供することを目的
とするものである。An object of the present invention is to provide a purification method for industrially obtaining high-quality acetic anhydride having a low content of diketene.
（問題点を解決するための手段） 本発明者は、工業的経済的有利に、ジケテン含有量の少
ない高品位の無水酢酸を得るための精製方法について鋭
意研究した。その結課、ジケテンを含有する原料粗無水
酢酸を紫外線照射処理することによって容易に高品質の
無水酢酸を得ることができるという事実を見出し、本発
明に到った。(Means for Solving Problems) The present inventor has earnestly studied a purification method for obtaining high-quality acetic anhydride having a small content of diketene, which is industrially and economically advantageous. As a result, they have found the fact that high-quality acetic anhydride can be easily obtained by subjecting raw material crude acetic anhydride containing diketene to ultraviolet irradiation, and arrived at the present invention.
また、原料粗無水酢酸中のジケテン含有量にもよるが、
この処理でやや着色する場合には、紫外線照射処理した
後に単蒸留程度の簡単な蒸留に付するか、または、紫外
線照射処理と同時に蒸留に付することによって、充分高
品位の無水酢酸を工業的、経済的有利に得ることができ
ることをも見出した。即ち、本発明は、ジケテンを含む
粗無水酢酸を紫外線照射処理し、必要に応じて該処理と
同時にあるいは該処理をした後に蒸留することを特徴と
する無水酢酸の精製方法である。Also, depending on the diketene content in the raw material crude acetic anhydride,
In the case of slightly coloring with this treatment, a sufficiently high-quality acetic anhydride can be industrially treated by subjecting it to simple distillation such as simple distillation after ultraviolet irradiation treatment, or by subjecting it to distillation at the same time as ultraviolet irradiation treatment. , Also found that it can be obtained economically. That is, the present invention is a method for purifying acetic anhydride, which comprises subjecting crude acetic anhydride containing diketene to ultraviolet irradiation treatment and, if necessary, distilling the crude acetic anhydride simultaneously with or after the treatment.
本発明に使用する紫外線照射の装置としては通常の市販
品が使用でき、形式的にも紫外線を外部から照射するも
の、内部に光源が設けてあるもの等いずれでもよい。As the apparatus for UV irradiation used in the present invention, an ordinary commercially available product can be used, and formally, it may be one that irradiates ultraviolet rays from the outside, one that internally has a light source, or the like.
また、紫外線の照射条件は無水酢酸中のジケテン等の含
有量処理液量、光源の出力および使用する装置の構造等
により適宜決められるが、概ね室温程度から無水酢酸の
沸点である１４０℃程度の間で、１〜80時間、照射処理
することによって、充分目的を達せられる。この処理で
やや着色するような場合には、その処理液を80トール程
度の減圧下で単蒸留に付するか、または、紫外線照射し
ながら所定の帯留時間が得られるように連続的に仕込
み、連続的に留出させる方法で処理できる。The irradiation conditions of ultraviolet rays are appropriately determined according to the content of diketene in acetic anhydride, the amount of the processing liquid, the output of the light source, the structure of the apparatus used, and the like. By performing the irradiation treatment for 1 to 80 hours, the purpose can be sufficiently achieved. In the case of slightly coloring in this treatment, the treatment liquid is subjected to simple distillation under a reduced pressure of about 80 Torr, or continuously charged so as to obtain a predetermined distillation time while irradiating with ultraviolet rays, It can be processed by a method of continuously distilling.
（発明の効果） 簡単な方法で経済的に無水酢酸中のジケテンを5PPM以下
（不検出）にまで除去することができる。得られた高品
質の無水酢酸は医農薬など精密化学分野原料として問題
なく使用することができる。(Effect of the invention) It is possible to economically remove diketene in acetic anhydride to 5 PPM or less (not detected) by a simple method. The obtained high-quality acetic anhydride can be used as a raw material for fine chemical fields such as medicine and agricultural chemicals without any problem.
以下に実施例を挙げて本発明の方法をさらに詳しく説明
する。Hereinafter, the method of the present invention will be described in more detail with reference to examples.
実施例−１ 原料粗無水酢酸500ｇをビーカーに入れ、スターラーで
撹拌しながら上部約１０cmより紫外線照射装置（（株）
長井製作所製10Ｗ，254nm）を用いて、室温下、約５時
間照射処理を行なった。Example 1 500 g of raw material crude acetic anhydride was placed in a beaker and stirred with a stirrer from an upper portion of about 10 cm to an ultraviolet irradiation device (Co., Ltd.).
Using Nagai Seisakusho 10 W, 254 nm), irradiation treatment was performed at room temperature for about 5 hours.
なお、本実験では、処理中に吸湿して無水酢酸が水と反
応し、酢酸になることを防止するために、乾燥窒素で空
気を置換したボックス中で実施した。また特に窒素でな
くとも乾燥空気中でも良い。処理装置が密閉式で、その
中に原料粗無水酢酸を入れその外部または内部に光源を
備えているものを用いるときは、蒸気吸湿防止対策は不
要である。In this experiment, in order to prevent acetic anhydride from reacting with water by absorbing moisture during the treatment and becoming acetic acid, the experiment was performed in a box in which air was replaced with dry nitrogen. Also, it is not particularly limited to nitrogen, but may be in dry air. When the treatment device is a closed type and the raw material crude acetic anhydride is put in the treatment device and a light source is provided outside or inside the treatment device, vapor moisture absorption prevention measures are not necessary.
本実験で処理した原料粗無水酢酸中のジケテンは250ppm
であり、処理液をガスクロマトグラフィーで分析した結
果は不検出（5ppm以下）であった。The raw material crude acetic anhydride treated in this experiment contained 250 ppm of diketene.
The result of gas chromatographic analysis of the treatment liquid was undetected (5 ppm or less).
実施例−２ 実施例−１と同じ方法で原料粗無水酢酸500ｇを７０時
間処理し、１０時間ごとにガスクロマトグラフィーで分
析した結果は表−１の通りであった。表−１から明らか
のように、処理時間とともにジケテンは少なくなり、７
０時間では不検出となった。しかし７０時間処理したも
のは、わずかに着色が認められた。これを100トーク減
圧下で単蒸留して、無色の無水酢酸を得た。このものを
ガスクロマトグラフィーで分析した結果ジケテンは不検
出であった。Example-2 In the same manner as in Example-1, 500 g of raw material crude acetic anhydride was treated for 70 hours and analyzed by gas chromatography every 10 hours. The results are shown in Table-1. As is clear from Table-1, diketene decreases with the processing time,
It was not detected at 0 hours. However, the one treated for 70 hours was slightly colored. This was subjected to simple distillation under reduced pressure of 100 talks to obtain colorless acetic anhydride. As a result of analyzing this product by gas chromatography, diketene was not detected.
Claims (1)
理し、必要に応じて該処理と同時にあるいは該処理をし
た後に蒸留することを特徴とする無水酢酸の精製方法。1. A method for purifying acetic anhydride, which comprises subjecting crude acetic anhydride containing diketene to ultraviolet irradiation treatment and, if necessary, distilling with or after the treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8277486A JPH0615492B2 (en) | 1986-04-10 | 1986-04-10 | Purification method of acetic anhydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8277486A JPH0615492B2 (en) | 1986-04-10 | 1986-04-10 | Purification method of acetic anhydride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62246537A JPS62246537A (en) | 1987-10-27 |
| JPH0615492B2 true JPH0615492B2 (en) | 1994-03-02 |
Family
ID=13783775
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8277486A Expired - Lifetime JPH0615492B2 (en) | 1986-04-10 | 1986-04-10 | Purification method of acetic anhydride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0615492B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9715318D0 (en) * | 1997-07-22 | 1997-09-24 | Bp Chem Int Ltd | Decolourisation process |
| US20230234975A1 (en) * | 2020-05-15 | 2023-07-27 | Tokuyama Corporation | Method for purifying organic compound and method for producing organic compound |
-
1986
- 1986-04-10 JP JP8277486A patent/JPH0615492B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62246537A (en) | 1987-10-27 |
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