JPS5822477B2 - Styrene sulfone - Google Patents
Styrene sulfoneInfo
- Publication number
- JPS5822477B2 JPS5822477B2 JP50061912A JP6191275A JPS5822477B2 JP S5822477 B2 JPS5822477 B2 JP S5822477B2 JP 50061912 A JP50061912 A JP 50061912A JP 6191275 A JP6191275 A JP 6191275A JP S5822477 B2 JPS5822477 B2 JP S5822477B2
- Authority
- JP
- Japan
- Prior art keywords
- purity
- styrene
- purification
- sulfonic acid
- metal salt
- 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
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
【発明の詳細な説明】
本発明は、スチレンスルホン酸金属塩、すなわち一般式
（式中、Ｍはアルカリ金属およびアルカリ土類金属であ
る）
で表わされる化合物の精製法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a process for the purification of metal styrene sulfonates, compounds of the general formula: where M is an alkali metal and an alkaline earth metal.
前記二股式を有するスチレンスルホン酸金属塩を製造す
る方法は、すでに知られている（米国特許第２５２７３
００号明細書、特公昭３５−１４２２０号および同３８
−２０５７０号明細書参照）。A method for producing styrene sulfonic acid metal salts having the bifurcated structure is already known (US Pat. No. 25,273).
Specification No. 00, Japanese Patent Publication No. 35-14220 and No. 38
-20570 specification).
しかし、これらの公知方法で製造されたスチレンスルホ
ン酸金属塩の純度はかなり低（、これらの方法には次の
ような欠点があって、工業的には満足できるものとはい
えない。However, the purity of the styrene sulfonic acid metal salts produced by these known methods is quite low (and these methods have the following drawbacks and cannot be said to be industrially satisfactory.
（１）製品が着色しがちである。(1) The product tends to be colored.
（２）スルホン化工程で副反応による水不溶性成分が多
量に生成し、それが最終製品に混入し、品質を低下させ
る。(2) In the sulfonation step, a large amount of water-insoluble components are generated due to side reactions, which are mixed into the final product and deteriorate its quality.
（３）脱・・ロジン化水素で生成する金属・・ロジン化
物を多量に含み、純度の低いものとなる。(3) Deletion: Metals produced by hydrogen rosination: Contains a large amount of rosin compounds, resulting in low purity.
本発明者らは、これらの欠点を克服した高純度スチレン
スルホン酸金属塩を得るために精製法について種々研究
を行なった結果、本発明を完成するにいたった。The present inventors conducted various studies on purification methods in order to obtain a high purity styrene sulfonic acid metal salt that overcomes these drawbacks, and as a result, completed the present invention.
以下本発明をさらに詳細に説明する。The present invention will be explained in more detail below.
すなわち、本発明者等は、公知法によって合成した低純
度のスチレンスルホン酸金属塩を有機溶媒を使用して精
製する方法を種々研究した結果、アセトン又はメタノー
ルと水の混合溶媒で精製スれば、金属ハロゲン化物の混
入率が５％以下、水不溶物を含まない高純度スチレンス
ルホン酸金属塩を得ることができることがわかった。That is, as a result of various researches on methods for purifying low-purity styrene sulfonic acid metal salts synthesized by known methods using organic solvents, the present inventors found that purification using a mixed solvent of acetone or methanol and water It has been found that it is possible to obtain a highly pure styrene sulfonic acid metal salt having a metal halide contamination rate of 5% or less and containing no water-insoluble matter.
本発明において使用する有機溶媒としては、脂肪族アル
コールＣｎＨ２ｎ＋１０Ｈ（ｎ−１〜４）、例えばメタ
ノール、エタノール、プロパツールおよびブタノール：
脂肪族ケトンＲ１ＣＯＲ２（Ｒ１および馬は水素または
炭素数１〜２個のアルキル基）、例えばアセトン、メチ
ルエチルケトン；および脂肪族エーテル例えばジオキサ
ンが挙げられる。Organic solvents used in the present invention include aliphatic alcohols CnH2n+10H (n-1 to 4), such as methanol, ethanol, propatool and butanol:
Aliphatic ketones R1COR2 (R1 and H are hydrogen or alkyl groups having 1 to 2 carbon atoms) such as acetone, methyl ethyl ketone; and aliphatic ethers such as dioxane.
本発明の有機溶媒・水混合系の混合比は、メタノールま
たはアセトンと水の混合物の場合に、一般に有機溶媒２
０〜９０％の混合物が使用できるが、７０〜８０％の混
合物が最も好ましい。The mixing ratio of the organic solvent/water mixture system of the present invention is generally such that when a mixture of methanol or acetone and water is used, the organic solvent:
Mixtures from 0 to 90% can be used, but mixtures from 70 to 80% are most preferred.
また、低純度スチレンスルホン酸金属塩を有機溶媒・水
混合系で精製するに当っては、該金属塩を有機溶媒・水
混合系中で６０°Ｃ１好ましくは４０〜５０°Ｃで攪拌
しながら溶解し、塩化カリウム等の不溶解残さを熱間ろ
過した後、ろ液をかきまぜながら冷却する。In addition, when purifying a low-purity styrene sulfonic acid metal salt in an organic solvent/water mixed system, the metal salt is stirred at 60°C, preferably 40 to 50°C, in an organic solvent/water mixed system. After dissolving and hot-filtering undissolved residues such as potassium chloride, the filtrate is cooled while stirring.
こうして析出するスチレンスルホン酸塩の純度は９５％
以上であり、精製収率も高い。The purity of the styrene sulfonate thus precipitated is 95%.
The results are as follows, and the purification yield is also high.
実施例 １
公知法によって合成した、スチレンスルホン酸カリウム
を０．７７４モル含む低純度品３４５グを７０％メタノ
ール・水（重量％）混合溶媒３８３グに添加し、４０〜
５０℃に加温して攪拌するとスチレンスルホン酸カリウ
ムは溶解し、不純物とＫして含まれる塩化カリウムは不
溶分として残る。Example 1 345 g of a low-purity product containing 0.774 mol of potassium styrene sulfonate synthesized by a known method was added to 383 g of a 70% methanol/water (wt%) mixed solvent.
When heated to 50° C. and stirred, potassium styrene sulfonate is dissolved, and potassium chloride, which is included as an impurity, remains as an insoluble component.
ここで熱濾過をして不溶分を派別して、沢液を攪拌下に
冷却すると、スチレンスルホン酸カリウムの白色結晶が
鱗片状として析出する。When the insoluble matter is removed by hot filtration and the resulting solution is cooled while stirring, white crystals of potassium styrene sulfonate are precipitated in the form of scales.
この結晶を理数して分析したところ純度９５％、精製収
率８０％であった。Physical and mathematical analysis of this crystal revealed that the purity was 95% and the purification yield was 80%.
実施例 ２〜４
精製溶媒を変えるほかは、実施例１と同一の条件で精製
したところ、えもれたスチレンスルホン・酸カリウムの
結晶は白色で沢過性がよ（、その純度がよび精製収率は
次のとおりであった。Examples 2 to 4 Purification was carried out under the same conditions as in Example 1 except for changing the purification solvent. The rates were as follows.
実施例 ５
使用低純度スチレンスルホン酸金属塩をカリウム塩から
ナトリウム塩に変えるほかは実施例１と同一の条件で精
製したところ、えられたスチレンスルホン酸ナトリウム
の結晶は白色で、純度９５％、精製収率７７％であった
。Example 5 Purification was carried out under the same conditions as in Example 1 except that the low-purity styrene sulfonate metal salt used was changed from potassium salt to sodium salt. The obtained sodium styrene sulfonate crystals were white and had a purity of 95%. The purification yield was 77%.
Claims (1)
系で精製することを特徴とするスチレンスルホン酸金属
塩の精製法。1. A method for purifying styrene sulfonic acid metal salt, which comprises purifying low-purity styrene sulfonate metal salt in an organic solvent/water mixture system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP50061912A JPS5822477B2 (en) | 1975-05-26 | 1975-05-26 | Styrene sulfone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP50061912A JPS5822477B2 (en) | 1975-05-26 | 1975-05-26 | Styrene sulfone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS51138646A JPS51138646A (en) | 1976-11-30 |
| JPS5822477B2 true JPS5822477B2 (en) | 1983-05-09 |
Family
ID=13184837
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP50061912A Expired JPS5822477B2 (en) | 1975-05-26 | 1975-05-26 | Styrene sulfone |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5822477B2 (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS514140A (en) * | 1974-06-27 | 1976-01-14 | Toyo Soda Mfg Co Ltd | Pp suchirensurupponsantanryotaimataha jugotaino seizohoho |
-
1975
- 1975-05-26 JP JP50061912A patent/JPS5822477B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS51138646A (en) | 1976-11-30 |
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