JPH05170680A - Production of sodium t-butoxide - Google Patents
Production of sodium t-butoxideInfo
- Publication number
- JPH05170680A JPH05170680A JP35644691A JP35644691A JPH05170680A JP H05170680 A JPH05170680 A JP H05170680A JP 35644691 A JP35644691 A JP 35644691A JP 35644691 A JP35644691 A JP 35644691A JP H05170680 A JPH05170680 A JP H05170680A
- Authority
- JP
- Japan
- Prior art keywords
- tba
- sodium
- reaction
- hydrocarbon solvent
- metallic sodium
- 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
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は化学工業薬品として有用
なナトリウム ｔ−ブトキシドの製造方法に関する。FIELD OF THE INVENTION The present invention relates to a method for producing sodium t-butoxide useful as a chemical industrial chemical.
【０００２】[0002]
【従来の技術】ナトリウムアルコキシドは、化学工業に
おいて、アルカリ性薬品として比較的多く使われて来
た。特に第１，第２アルコールのアルコキシドは、金属
ナトリウムとの反応性が良いので、比較的簡単に高純度
のアルコキサイドを得る事ができ、比較的に多く使われ
て来た。しかしながら、第３アルコールのアルコキシド
の場合は、アルコールが金属ナトリウムと反応するより
も、既に生成したアルコキシドと錯体を形成し、安定化
して、金属ナトリウムと反応しなくなる為に、高純度、
高収率のアルコキシドを得る事は著しく困難であった。
特にｔ−ブチルアルコールの場合融点が２６℃と高いた
め、コンデンサー内で結晶が析出したりし、取扱いにく
い製品であった。BACKGROUND OF THE INVENTION Sodium alkoxide has been used relatively frequently as an alkaline chemical in the chemical industry. In particular, the alkoxides of the primary and secondary alcohols have good reactivity with metallic sodium, so that high-purity alkoxide can be obtained relatively easily and have been used relatively often. However, in the case of an alkoxide of a tertiary alcohol, the alcohol forms a complex with the already-formed alkoxide and stabilizes and does not react with metallic sodium, rather than reacting with the metallic sodium.
It was extremely difficult to obtain a high yield of alkoxide.
In particular, in the case of t-butyl alcohol, the melting point was as high as 26 ° C., so that crystals were precipitated in the capacitor and the product was difficult to handle.
【０００３】第３アルコールのアルコキシドの製造方法
としては特開昭５２−１５３９０４号に不活性炭化水素
溶媒中、オートクレーブ中、９８〜１６０℃の温度範囲
でナトリウム分散体を使用して反応させることが開示さ
れている。As a method for producing an alkoxide of a tertiary alcohol, JP-A No. 52-153904 discloses a reaction using a sodium dispersion in an inert hydrocarbon solvent in an autoclave at a temperature range of 98 to 160 ° C. It is disclosed.
【０００４】[0004]
【課題を解決するための手段】本発明は炭化水素系溶媒
を５〜１５重量％含有させたｔ−ブチルアルコール溶液
中、撹拌下、溶融した金属ナトリウムを噴霧し、微粒子
化させて反応させることを特徴とするナトリウム ｔ−
ブトキシドの製造方法である。Means for Solving the Problems The present invention comprises spraying molten metallic sodium in a t-butyl alcohol solution containing a hydrocarbon solvent in an amount of 5 to 15% by weight to form fine particles for reaction. Sodium t-
It is a method for producing butoxide.
【０００５】本発明に用いる炭化水素系溶媒としてはｎ
−ヘキサンやイソオクタン等の脂肪族炭化水素あるいは
トルエンやキシレン等の芳香族炭化水素もしくはそれら
の混合物が挙げられるが、取扱いやすさの点でｎ−ヘキ
サンが好しい。The hydrocarbon solvent used in the present invention is n
Examples thereof include an aliphatic hydrocarbon such as hexane and isooctane, an aromatic hydrocarbon such as toluene and xylene, or a mixture thereof, and n-hexane is preferable from the viewpoint of easy handling.
【０００６】本発明を実施するためにはｔ−ブチルアル
コール（ＴＢＡ）を３０〜５０℃に加熱、ＴＢＡを溶解
し、炭化水素系溶媒と混合し、強く撹拌する。この溶液
中に窒素気流下、溶融した金属ナトリウムを噴霧し、仕
込終了後、還流下、反応排ガス中の水素ガスが検出され
なくなるまで反応させる。反応終了後、溶媒及び過剰の
ＴＢＡを留去し、ナトリウム ｔ−ブトキシドを得る。
この際、留去する温度を調節することによりアルコール
付加体（ＮａＯＣ4 Ｈ9 t ・Ｃ4 Ｈ9 t ＯＨ）あるいは
フリーのナトリウム ｔ−ブトキシド（ＮａＯＣ4 Ｈ9
t ）が得られる。In order to carry out the present invention, t-butyl alcohol (TBA) is heated to 30 to 50 ° C. to dissolve TBA, mix with a hydrocarbon solvent and stir vigorously. Molten metallic sodium is sprayed into this solution under a nitrogen stream, and after the completion of charging, the mixture is reacted under reflux until hydrogen gas in the reaction exhaust gas is no longer detected. After completion of the reaction, the solvent and excess TBA are distilled off to obtain sodium t-butoxide.
At this time, an alcohol adduct (NaOC 4 H 9 t · C 4 H 9 t OH) or free sodium t-butoxide (NaOC 4 H 9
t ) is obtained.
【０００７】ＴＢＡと金属ナトリウムとの量は特に制限
はないが、ＴＢＡの量が少いと反応時間が長くなり、ま
た、多いと大きな反応槽が必要あるいは反応終了後、過
剰のＴＢＡの留去に時間がかかる等の問題があり、通常
は、金属ナトリウムに対し、３０〜８０倍重量、好しく
は５５〜６５倍重量のＴＢＡを使用して反応させる。The amounts of TBA and metallic sodium are not particularly limited, but if the amount of TBA is small, the reaction time becomes long, and if it is large, a large reaction tank is required or excess TBA is distilled off after the reaction is completed. There is a problem that it takes time, and usually, 30 to 80 times by weight, preferably 55 to 65 times by weight, of TBA is used to react with metallic sodium.
【０００８】[0008]
【実施例】次に実施例を挙げて本発明を更に詳細に説明
する。 実施例１．アルコール溶解室で溶解したＴＢＡ、１５３
０kgおよびｎ−ヘキサン１７０kgを溶媒調製槽で調製
し、反応槽へ送った。反応槽に窒素を流し、反応槽を撹
拌した。１２５°〜１３０℃に溶融した金属ナトリウム
を１kg／分の割合で反応槽に噴霧し、仕込終了後、加熱
し、反応排ガス中の水素ガスが検出しなくなるまで還流
下反応させた（１０時間）。反応液を乾燥器に移送し、
液が全てなくなるまでｎ−ヘキサンおよび過剰のＴＢＡ
を留去した（内温９５℃）。乾燥器を振動させ、粉末の
ナトリウム ｔ−ブトキシドのアルコール付加体１７７
kgを得た。EXAMPLES Next, the present invention will be described in more detail with reference to examples. Example 1. TBA dissolved in an alcohol dissolution chamber, 153
0 kg and 170 kg of n-hexane were prepared in a solvent preparation tank and sent to the reaction tank. The reaction tank was flushed with nitrogen and the reaction tank was stirred. Metallic sodium melted at 125 ° to 130 ° C was sprayed into the reaction tank at a rate of 1 kg / min, heated after completion of the charging, and reacted under reflux until hydrogen gas in the reaction exhaust gas was no longer detected (10 hours). .. Transfer the reaction solution to the dryer,
N-hexane and excess TBA until all liquid is gone
Was distilled off (internal temperature: 95 ° C.). Vibrate the drier and add powdered sodium t-butoxide alcohol adduct 177.
got kg.
【０００９】[0009]
【発明の効果】本発明の製造方法はＴＢＡに対し５〜１
５％の炭化水素系溶媒を添加することにより、ＴＢＡ
の固結温度を下げ、取扱いを用意する共沸によりコン
デンサー内のＴＢＡの固結を防止し、還流条件での反応
を容易にしたこと、さらに金属ナトリウムを溶融、噴霧
し、微粒子化させることにより、取扱いにくいナトリウ
ム分散体を使用せず、しかも常圧での反応を可能したこ
と等、工業的に優れた製造方法である。The production method of the present invention is 5 to 1 with respect to TBA.
By adding 5% hydrocarbon solvent, TBA
By lowering the solidification temperature of TBA and azeotropically preparing for handling, TBA in the condenser was prevented from solidifying, and the reaction under reflux conditions was facilitated. Further, by melting and spraying metallic sodium, it was made into fine particles. In addition, it is an industrially excellent manufacturing method in that it is possible to carry out the reaction under normal pressure without using a sodium dispersion which is difficult to handle.
Claims (2)
せたｔ−ブチルアルコール溶液中、撹拌下、溶融した金
属ナトリウムを噴霧し、微粒子化させて反応させること
を特徴とするナトリウム ｔ−ブトキシドの製造方法。1. A sodium t-characterized by spraying molten metal sodium in a t-butyl alcohol solution containing a hydrocarbon solvent in an amount of 5 to 15% by weight with stirring to atomize and react. Butoxide production method.
求項１の製造方法。2. The method according to claim 1, wherein the hydrocarbon solvent is n-hexane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35644691A JPH05170680A (en) | 1991-12-25 | 1991-12-25 | Production of sodium t-butoxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35644691A JPH05170680A (en) | 1991-12-25 | 1991-12-25 | Production of sodium t-butoxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05170680A true JPH05170680A (en) | 1993-07-09 |
Family
ID=18449052
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35644691A Pending JPH05170680A (en) | 1991-12-25 | 1991-12-25 | Production of sodium t-butoxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05170680A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6437198B1 (en) | 1998-06-12 | 2002-08-20 | Basf Aktiengesellschaft | Method for producing alkali metal alcoholates |
| JP2003514882A (en) * | 1999-11-24 | 2003-04-22 | ヒェメタル ゲゼルシャフト ミット ベシュレンクテル ハフツング | Concentrated stable alkali alcoholate solution |
| JP2006122864A (en) * | 2004-11-01 | 2006-05-18 | Nippon Soda Co Ltd | Apparatus and method for atomizing metallic sodium |
| CN107602346A (en) * | 2017-09-07 | 2018-01-19 | 安徽省化工设计院 | A kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes |
| CN112250543A (en) * | 2020-09-18 | 2021-01-22 | 安徽金邦医药化工有限公司 | Production process of medicinal raw material sodium methoxide |
-
1991
- 1991-12-25 JP JP35644691A patent/JPH05170680A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6437198B1 (en) | 1998-06-12 | 2002-08-20 | Basf Aktiengesellschaft | Method for producing alkali metal alcoholates |
| JP2003514882A (en) * | 1999-11-24 | 2003-04-22 | ヒェメタル ゲゼルシャフト ミット ベシュレンクテル ハフツング | Concentrated stable alkali alcoholate solution |
| JP2006122864A (en) * | 2004-11-01 | 2006-05-18 | Nippon Soda Co Ltd | Apparatus and method for atomizing metallic sodium |
| CN107602346A (en) * | 2017-09-07 | 2018-01-19 | 安徽省化工设计院 | A kind of metallic sodium Division A League Matches of French Football sodium alkoxide continuous production processes |
| CN112250543A (en) * | 2020-09-18 | 2021-01-22 | 安徽金邦医药化工有限公司 | Production process of medicinal raw material sodium methoxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH05170680A (en) | Production of sodium t-butoxide | |
| JP2002332251A (en) | Method for producing halogen-substituted dibenzyl alcohol, halogen-substituted dibenzyl alcohol and use thereof | |
| US6444190B2 (en) | Reduction compositions and processes for making the same | |
| CA1072573A (en) | Process for the preparation of orthosilicic acid tetra-alkoxyalkyl esters | |
| CN113880875B (en) | Synthesis method of triethylsilane | |
| JPH08259212A (en) | Method for synthesizing disilicon hexafluoride | |
| JP3386860B2 (en) | Method for producing N-hydroxy-N'-diazenium oxide | |
| JPH07278156A (en) | Preparation of dimethylamine - borane | |
| CN117550981B (en) | Preparation method of 2-amino-5-fluoro acetophenone | |
| US20030023105A1 (en) | Synthesis and isolation of metal alkoxides | |
| WO2024021190A1 (en) | Method for preparing phosphine-based compound and use thereof | |
| JP3779452B2 (en) | Method for producing alcohols | |
| US4246176A (en) | Synthesis of 5-aroyl-1-hydrocarbylpyrrole-2-acetic acid | |
| JPS6391392A (en) | Production of soluble metal alkoxide from low solubility reactant | |
| WO1997005879A1 (en) | Reductions using hydrides | |
| US2964379A (en) | Preparation of alkali metal phosphides | |
| WO1998013319A1 (en) | Novel reduction compositions and processes for making the same | |
| CS222659B2 (en) | Method of making the alcoxyalanate of the metals of alcalic soils | |
| EP0703233A2 (en) | Process for the preparation of 5-substituted-1-azabicyclo (3.3.0) octanes | |
| JP2961266B1 (en) | Method for producing tetrafluorohydrazine | |
| CN114805176A (en) | Preparation method of 6, 6-dimethyl-3-azabicyclo [3.1.0] hexane | |
| JPH05506641A (en) | Production of 2,2-dialkoxycyclic orthoester derived from lactone | |
| JPH03275502A (en) | Production of sodium borohydride | |
| JPH09110774A (en) | Production of 1,1-dialkoxycycloalkane | |
| JPH0229053B2 (en) |