JPS6143629A - Method for purifying polyether - Google Patents
Method for purifying polyetherInfo
- Publication number
- JPS6143629A JPS6143629A JP16428584A JP16428584A JPS6143629A JP S6143629 A JPS6143629 A JP S6143629A JP 16428584 A JP16428584 A JP 16428584A JP 16428584 A JP16428584 A JP 16428584A JP S6143629 A JPS6143629 A JP S6143629A
- Authority
- JP
- Japan
- Prior art keywords
- polyether
- exchange resin
- cation exchange
- water
- polypropylene glycol
- 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
- Polyethers (AREA)
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） −本発明は、ポリエーテルの精製法に関する。[Detailed description of the invention] (Industrial application field) - The present invention relates to a method for purifying polyether.
更に詳しくは、着色したポリエーテルの脱色法に関する
。More specifically, the present invention relates to a method for decolorizing colored polyether.
（従来の技術および発明が解決しようとする問題点）
ポリエーテルは、通常、アルキレンオキサイドをアルコ
ール類等に付加させて製造される。その製造時、後処理
時または保存中に加熱、空気酸化、あるいは安定剤等の
添加物の変色等により、元来色調の淡いはずのポリエー
テルが着色し、製品として問題となる。この着色の傾向
は、特に、塩基性触媒により製造されたものにはなはだ
しい。(Prior art and problems to be solved by the invention) Polyethers are usually produced by adding alkylene oxide to alcohols and the like. Polyether, which is originally light in color, becomes colored due to heating, air oxidation, or discoloration of additives such as stabilizers during production, post-processing, or storage, causing problems as a product. This coloring tendency is particularly severe in those produced using basic catalysts.
ところで、このように着色したポリエーテルの脱色方法
としては活性炭を使用する方法があるが、この方法では
ポリエーテルが高粘度でありｐ過がうまく行なえないば
かりか脱色が充分でな（、ポリエーテルの種類によって
は逆に着色度が増す場合もあり問題である。また、粘度
を低下させるために水や溶媒を使用することもできるが
、活性炭を使用した場合においては見た目には脱色でき
ているようであっても、脱溶媒してみるとほとんど処理
前と同程度の着色度であるという問題もある。By the way, there is a method for decolorizing polyether that has been colored in this way, using activated carbon, but with this method, the polyether has a high viscosity, and p-filtration cannot be carried out well, and the decolorization is not sufficient. Depending on the type of carbon, the degree of coloration may increase, which is a problem.Also, water or a solvent can be used to reduce the viscosity, but when activated carbon is used, the color can be visually removed. However, there is a problem in that when the solvent is removed, the degree of coloring is almost the same as before treatment.
したがって、ポリエーテルの脱色という点からの精製に
は活性炭を使用できないのが実情である。Therefore, the reality is that activated carbon cannot be used to purify polyether from the standpoint of decolorizing it.
本発明の目的は着色したポリエーテルの効果的な精製法
を提供することにある。It is an object of the present invention to provide an effective method for purifying colored polyethers.
（問題点を解決するだめの手段）
本発明者らは、上記目的を達成するため鋭意検討し、ポ
リエーテルを水の存在下に陽イオン交換樹脂で処理する
ことにより脱色できることを見出し、本発明を完成した
。(Means for Solving the Problems) In order to achieve the above object, the present inventors have made extensive studies and found that polyether can be decolored by treating it with a cation exchange resin in the presence of water. completed.
すなわち、本発明は、ポリエーテルを水の存在下に陽イ
オン交換樹脂で処理することを特徴とするポリエーテル
の精製法である。That is, the present invention is a polyether purification method characterized by treating polyether with a cation exchange resin in the presence of water.
本発明の方法を適用できるポリエーテルとは、活性水素
化合物にアルキレンオキサイドを付加して得られるもの
である。The polyether to which the method of the present invention can be applied is one obtained by adding alkylene oxide to an active hydrogen compound.
ここにいう活性水素化合物としてはメタノール、エタノ
ール、オクタツール、フェノール、ノニルフェノール等
の一価のアルコールまたはフェノール類、エチレングリ
コール、プロピレングリコール、１，４−ブタンジオー
ル等の二価ｆ７）７＃：＋−ル類、トリメチロールプロ
パン、ペンタエリスリトール、ンルビトール、ソルビタ
ン、糖類等の多価アルコール類、アニリン、エチレンジ
アミン、ジエチレントリアミン、トン′エンジアミン、
ジエチルアミン等のアミン化合物などがあげられる。The active hydrogen compounds mentioned here include monohydric alcohols or phenols such as methanol, ethanol, octatool, phenol, and nonylphenol, and divalent f7)7#:+ such as ethylene glycol, propylene glycol, and 1,4-butanediol. polyhydric alcohols such as alcohols, trimethylolpropane, pentaerythritol, nlubitol, sorbitan, sugars, aniline, ethylenediamine, diethylenetriamine, ton'enediamine,
Examples include amine compounds such as diethylamine.
また、アルキレンオキサイドとしてはエチレンオキサイ
ド、プロピレンオキサイド、スチレンオキサイド等があ
げられる。これらのアルキレンオキサイドは一種または
二種以上が用いられる。これらのアルキレンオキサイド
の付加量は目的により異なり限定することはできないが
、通常、活性水素化合物１モル当り５〜１６モルである
。Furthermore, examples of the alkylene oxide include ethylene oxide, propylene oxide, and styrene oxide. One or more types of these alkylene oxides may be used. The amount of these alkylene oxides added varies depending on the purpose and cannot be limited, but is usually 5 to 16 moles per mole of active hydrogen compound.
本発明の方法に使用する陽イオン交換樹脂としては、通
常、市販のものが問題なく使用でき、そのイオン型とし
てはＨ型のものが好ましい。As the cation exchange resin used in the method of the present invention, commercially available cation exchange resins can be used without any problems, and the H type is preferable as the ion type.
本発明の方法においては、陽−イオン交換樹脂で処理す
るポリエーテル中には水が添加されていることが必要で
あり、その添加量としてはポリエーテルに対して１〜１
０重量％、好ましくは２〜５重量％である。水の添加量
が１重量％未満では脱色が５まく行なえないことがあり
、また１０重量％を超えるとそれ以下と比べ脱色性にほ
とんど差がな（、脱水に時間がかかり実際的でない。In the method of the present invention, it is necessary to add water to the polyether treated with the cation exchange resin, and the amount of water added is 1 to 1
0% by weight, preferably 2-5% by weight. If the amount of water added is less than 1% by weight, decolorization may not be possible, and if it exceeds 10% by weight, there is almost no difference in decolorization compared to less than 10% by weight (dehydration takes a long time and is not practical).
処理温度は室温から樹脂の可使用温度の間であればいづ
れでもよいがポリエーテルの粘度を勘案して最適の温度
が決められる、通常、６０〜９０℃が適当である。The treatment temperature may be any temperature between room temperature and the usable temperature of the resin, but the optimum temperature is determined by taking into account the viscosity of the polyether, and is usually 60 to 90°C.
処理時間は、とくに制限されないが、あまり長時間であ
るとポリエーテル中に含まれる塩基性物質が除去され、
ポリエーテルの性質が変わってしまう恐れがあると共に
色調改善にも悪い影響がでることがあり、可能な限り短
かい方がよい。The treatment time is not particularly limited, but if the treatment time is too long, the basic substances contained in the polyether will be removed.
It is better to keep it as short as possible since there is a risk that the properties of the polyether may change and color tone improvement may also be adversely affected.
処理の方法には制限はないが、通常カラム法が好ましく
、この際の流液量としてはＳ■（空間速度）５〜１５、
好ましくは５〜９が適当である。Although there are no restrictions on the treatment method, a column method is usually preferred, and the flow rate in this case is S■ (space velocity) 5 to 15,
Preferably 5 to 9 is appropriate.
（実施例） 以下、実施例により本発明を説明する。(Example) The present invention will be explained below with reference to Examples.
実施例−１
色調茶褐色、水酸基価５５６■ＫＯＨ／Ｐのポリプロピ
レングリコールを攪拌機付の５００ゴフラスコに取り水
６重量％を添加する。窒素気流下で攪拌しながら温度６
０〜７０℃にあげる。陽イオン交換樹脂を詰めたカラム
に硫量ＳＶ６．６．２．４および１．６の速度でそれぞ
れ通した。流出したポリプロピレングリコールな減圧脱
水した結果、色調、水酸基価、ＰＨおよび水分がそれぞ
れ表−１に示すポリプロピレングリコールが得られた。Example 1 Polypropylene glycol having a brown color and a hydroxyl value of 556 ■KOH/P was placed in a 500 Go flask equipped with a stirrer, and 6% by weight of water was added thereto. Temperature 6 while stirring under nitrogen flow
Raise to 0-70℃. It was passed through a column packed with cation exchange resin at a rate of sulfur content SV 6.6.2.4 and 1.6, respectively. As a result of dehydrating the polypropylene glycol that flowed out under reduced pressure, polypropylene glycol having the color tone, hydroxyl value, pH, and water content shown in Table 1 was obtained.
実施例−２
色調黒褐色、水酸基価４４７■ＫＯＨ／ｒのポリプロピ
レングリコールを実施例−１のように前処理を行ない、
陽イオン交換樹脂を詰めたカラムに流量ｓＶ９．０の速
度で通す。流出したポリプロピレングリコールを減圧脱
水した結果、色調、水酸基価、ＰＨおよび水分が表−１
に示すポリエーテルが得られた。Example-2 Polypropylene glycol having a dark brown color and a hydroxyl value of 447 KOH/r was pretreated as in Example-1,
It is passed through a column packed with cation exchange resin at a flow rate of sV 9.0. As a result of dehydrating the spilled polypropylene glycol under reduced pressure, the color tone, hydroxyl value, pH, and water content are shown in Table 1.
A polyether shown in was obtained.
比較例−１
実施例−１で使用したポリプロピレングリコールを陰イ
オン交換樹脂を詰めたカラムに流量Ｓ Ｖ ５．７、６
．４の速度でそれぞれ通した。流出したポリプロピレン
グリコールを減圧脱水した結果、色調、水酸基価、ＰＨ
および水分がそれぞれ表−１に示すポリプロピレングリ
コールが得られた。色調は劣化の方向であった。Comparative Example-1 The polypropylene glycol used in Example-1 was put into a column packed with anion exchange resin at a flow rate of SV 5.7, 6.
．． I passed each at a speed of 4. As a result of dehydrating the polypropylene glycol that flowed out under reduced pressure, the color tone, hydroxyl value, and pH were determined.
A polypropylene glycol having a moisture content shown in Table 1 was obtained. The color tone was in the direction of deterioration.
比較例−２〜５
実施例−２に使用し、たポリプロピレングリコールな表
−２に示す活性炭、過酸化水素、活性白土、およびボロ
ンハイドライドでそれぞれ処理したがいづれも効果がな
かった。結果を表−２に示す。Comparative Examples 2 to 5 The polypropylene glycol used in Example 2 was treated with activated carbon, hydrogen peroxide, activated clay, and boron hydride shown in Table 2, but none of them had any effect. The results are shown in Table-2.
Claims (2)
処理することを特徴とするポリエーテルの精製法。(1) A method for purifying polyether, which comprises treating polyether with a cation exchange resin in the presence of water.
サイドを付加したものである特許請求の範囲第１項記載
の方法。(2) The method according to claim 1, wherein the polyether is a polyhydric alcohol with an alkylene oxide added thereto.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16428584A JPS6143629A (en) | 1984-08-07 | 1984-08-07 | Method for purifying polyether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16428584A JPS6143629A (en) | 1984-08-07 | 1984-08-07 | Method for purifying polyether |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6143629A true JPS6143629A (en) | 1986-03-03 |
| JPH0449853B2 JPH0449853B2 (en) | 1992-08-12 |
Family
ID=15790193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16428584A Granted JPS6143629A (en) | 1984-08-07 | 1984-08-07 | Method for purifying polyether |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6143629A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01185323A (en) * | 1988-01-18 | 1989-07-24 | Sakamoto Yakuhin Kogyo Kk | Production of high-molecular weight flame-retardant |
| US5342541A (en) * | 1989-03-29 | 1994-08-30 | The Dow Chemical Company | Purified hydroxy-functional polyether compounds |
| US7495063B2 (en) | 2006-02-03 | 2009-02-24 | Dow Global Technologies Inc. | Reduced oligomer concentration in high purity polyalkylene glycols |
| CN105131274A (en) * | 2015-08-20 | 2015-12-09 | 西安蓝晓科技新材料股份有限公司 | Method for removing sodium ions in polytetrahydrofuran production |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5616524A (en) * | 1979-07-20 | 1981-02-17 | Mitsubishi Chem Ind Ltd | Purification of crude polytetramethylene glycol |
-
1984
- 1984-08-07 JP JP16428584A patent/JPS6143629A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5616524A (en) * | 1979-07-20 | 1981-02-17 | Mitsubishi Chem Ind Ltd | Purification of crude polytetramethylene glycol |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01185323A (en) * | 1988-01-18 | 1989-07-24 | Sakamoto Yakuhin Kogyo Kk | Production of high-molecular weight flame-retardant |
| US5342541A (en) * | 1989-03-29 | 1994-08-30 | The Dow Chemical Company | Purified hydroxy-functional polyether compounds |
| US7495063B2 (en) | 2006-02-03 | 2009-02-24 | Dow Global Technologies Inc. | Reduced oligomer concentration in high purity polyalkylene glycols |
| CN105131274A (en) * | 2015-08-20 | 2015-12-09 | 西安蓝晓科技新材料股份有限公司 | Method for removing sodium ions in polytetrahydrofuran production |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0449853B2 (en) | 1992-08-12 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |