JP3408575B2 - Dehydration method of tangible sodium hydrosulfide with inert gas - Google Patents
Dehydration method of tangible sodium hydrosulfide with inert gasInfo
- Publication number
- JP3408575B2 JP3408575B2 JP08603093A JP8603093A JP3408575B2 JP 3408575 B2 JP3408575 B2 JP 3408575B2 JP 08603093 A JP08603093 A JP 08603093A JP 8603093 A JP8603093 A JP 8603093A JP 3408575 B2 JP3408575 B2 JP 3408575B2
- Authority
- JP
- Japan
- Prior art keywords
- sodium hydrosulfide
- tangible
- dehydration
- inert gas
- dehydrating
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/38—Dehydration
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、水硫化ソーダのフレー
ク状、チップ状、ペレット状等の成型物や、水溶液の冷
却固化物を前記成型物と同程度まで粉砕した物など、あ
る大きさ以上の水硫化ソーダ有形物を脱水する方法に関
する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention has a certain size such as flakes, chips, pellets and the like of sodium hydrosulfide, and a product obtained by crushing a cooled and solidified solution of an aqueous solution to the same extent as the above-mentioned molded product. The present invention relates to a method for dehydrating tangible substances of sodium hydrosulfide.
【０００２】[0002]
【従来の技術】市販の水硫化ソーダは、全水硫化ソーダ
分が約２５〜４５％の水溶液を加熱濃縮して全水硫化ソ
ーダ分約７０重量％にし、この濃縮液をフレーカーにか
けてフレーク状にするか、容器に入れて冷却固化したも
のである。この水硫化ソーダには水分が２５％強含有さ
れており、水分を嫌う反応、特に有機物との反応などへ
の使用を妨げている。2. Description of the Related Art Commercially available sodium hydrosulfide is concentrated by heating an aqueous solution having a total sodium hydrosulfide content of about 25 to 45% to a total sodium hydrosulfide content of about 70% by weight, and the concentrated solution is flaked to form flakes. Or put in a container and cooled and solidified. This sodium hydrosulfide contains a little more than 25% of water, which hinders its use in reactions that hate water, especially in reactions with organic substances.
【０００３】一方、高濃度水硫化ソーダを脱水濃縮によ
って製造するときには、濃度７５重量％付近から液粘度
が急激に上昇し、液の移動を通常のポンプで行うことが
不可能になり、また、増粘にともない脱水効率も著しく
低下する。このような事情から水硫化ソーダは、７０〜
７５重量％のものが市販されている。On the other hand, when producing high-concentration sodium hydrosulfide by dehydration concentration, the liquid viscosity rapidly rises from a concentration of around 75% by weight, and it becomes impossible to move the liquid with an ordinary pump. Dehydration efficiency also decreases significantly as the viscosity increases. Under these circumstances, sodium hydrosulfide is 70-
75% by weight is commercially available.
【０００４】そこで、本発明者等は、水硫化ソーダ有形
物を減圧下で加熱脱水する方法として、減圧下で６０℃
以下の温度で有形物の表面を脱水した後、加熱脱水する
方法（特願平５−４１２６５号出願参照）や、水硫化ソ
ーダ有形物の溶融付着を防止するため、低水分の水硫化
ソーダ粉末を添加して加熱脱水する方法（特願平５−４
１２６７号出願参照）を先に提案した。Therefore, the inventors of the present invention, as a method of heating and dehydrating sodium hydrosulfide tangible material under reduced pressure, at 60 ° C. under reduced pressure.
A method of dehydrating the surface of a tangible material at the following temperature, followed by heating and dehydration (see Japanese Patent Application No. 5-41265) or a low-moisture content of sodium hydrosulfide powder in order to prevent melting and adhesion of a sodium hydrosulfide tangible material. Method of adding water to heat dehydration (Japanese Patent Application No. 5-4
No. 1267 application) was previously proposed.
【０００５】[0005]
【発明が解決しようとする課題】しかし、前者の方法
は、減圧下の予備的脱水における温度管理を厳密に行う
必要があり、かつ、脱水処理に時間がかかるため、その
間に空気中の酸素や蒸発水などに起因する水硫化ソーダ
の変質を避けることができない。また、後者の方法で
は、脱水した後有形物から粉末を篩別する工程が必要に
なり、また、添加する粉末は脱水処理済の有形物を粉砕
して用いるので、生産効率の低下につながるとともに、
粉砕操作中に空気と接触して変質した粉末が製品中に混
入する恐れがある。そこで、本発明は、上記の欠点を解
消し、水硫化ソーダ有形物を簡単に、短時間で脱水する
方法を提供しようとするものである。However, in the former method, it is necessary to strictly control the temperature in the preliminary dehydration under reduced pressure, and since the dehydration process takes time, oxygen in the air and Deterioration of sodium hydrosulfide caused by evaporating water is unavoidable. Also, in the latter method, a step of sieving the powder from the tangible material after dehydration is required, and the powder to be added is pulverized and used for the dehydrated tangible material, which leads to a decrease in production efficiency. ,
There is a risk that powder that has been altered by contact with air during the crushing operation may be mixed into the product. Therefore, the present invention is intended to solve the above-mentioned drawbacks and to provide a method for easily and quickly dehydrating sodium hydrosulfide tangible material.
【０００６】[0006]
【課題を解決するための手段】本発明は、(1) 全水硫化
ソーダ分６５重量％以上を含有する水硫化ソーダ有形物
を脱水する方法において、水硫化ソーダ有形物に不活性
ガスを流して有形物の表面を脱水した後、減圧下で加熱
脱水することを特徴とする水硫化ソーダ有形物の脱水方
法、(2) 原料の水硫化ソーダの融点プラス５℃以下の温
度に加熱された不活性ガスを、該原料１００ｇ当たり毎
分２ノルマルリットル以上の流量で流して有形物の表面
を脱水した後、１５トール以下の減圧下で加熱脱水する
ことを特徴とする上記(1) 記載の水硫化ソーダ有形物の
脱水方法、及び、(3) 水硫化ソーダ有形物原料１００ｇ
当たり毎分２ノルマルリットル以上の流量で不活性ガス
を流しながら、該原料を収容する容器を原料の水硫化ソ
ーダの融点プラス５℃以下の温度に加熱して有形物の表
面を脱水した後、１５トール以下の減圧下で加熱脱水す
ることを特徴とする上記(1) 記載の水硫化ソーダ有形物
の脱水方法である。Means for Solving the Problems The present invention provides (1) a method for dehydrating a sodium hydrosulfide tangible material containing a total sodium hydrosulfide content of 65% by weight or more, in which an inert gas is passed through the sodium hydrosulfide tangible material. Method of dehydrating sodium hydrosulfide tangible material, characterized in that the surface of the tangible material is dehydrated by heating and then dehydrated by heating under reduced pressure, (2) melting point of sodium hydrosulfide as a raw material plus heating to a temperature of 5 ° C or less The inert gas is flowed at a flow rate of 2 normal liters per minute or more per 100 g of the raw material to dehydrate the surface of the tangible material, and then heat dehydration is performed under a reduced pressure of 15 Torr or less. Sodium hydrosulfide tangible material dehydration method, and (3) Sodium hydrosulfide tangible material 100 g
After flowing an inert gas at a flow rate of 2 normal liters per minute or more per minute, the container containing the raw material is heated to the melting point of the raw material sodium hydrosulfide plus 5 ° C. or lower to dehydrate the surface of the tangible material, The method for dehydrating a tangible substance of sodium hydrosulfide according to the above (1), characterized in that the dehydration is carried out by heating under a reduced pressure of 15 Torr or less.
【０００７】本発明で、水硫化ソーダ有形物とは、フレ
ーク状、チップ状、ペレット状のもの、さらには水溶液
の冷却固化物を粉砕した約３〜１０ｍｍ径の粉砕物をい
う。また、本発明で用いる不活性ガスとしては、水硫化
ソーダに対して不活性な水素、窒素、アルゴンなどのガ
スを挙げることができる。本発明は、全水硫化ソーダ分
６５重量％以上の水硫化ソーダ有形物を脱水するのに有
効である。全水硫化ソーダ分が６５重量％を下回ると脱
水の過程で溶融し容器に付着し、脱水効率を低下させる
恐れがある。In the present invention, the tangible substance of sodium hydrosulfide refers to flakes, chips, pellets, and pulverized products obtained by pulverizing a cooled solidified product of an aqueous solution and having a diameter of about 3 to 10 mm. Further, examples of the inert gas used in the present invention include gases such as hydrogen, nitrogen, and argon that are inert to sodium hydrosulfide. INDUSTRIAL APPLICABILITY The present invention is effective for dehydrating a sodium hydrosulfide tangible substance having a total sodium hydrosulfide content of 65% by weight or more. If the total sodium hydrosulfide content is less than 65% by weight, it may melt during the dehydration process and adhere to the container, reducing the dehydration efficiency.
【０００８】[0008]
【作用】本発明者等は、水硫化ソーダの脱水方法を種々
検討する中で、水硫化ソーダ有形物を容器に入れて不活
性ガスを流しながら、比較的低温で脱水したところ、有
形物の表面が徐々に脱水されて白色化し、有形物表面に
低水分水硫化ソーダ被膜が形成されることを見出した。
この白色化現象は、不活性ガスの通気時間、加熱温度な
どにより、差があるものの、大気圧、室温で行うときに
は、不活性ガスの通気開始から約３分で白色化現象が現
れ、３０〜４０分で完全に白色化した。上記の低水分水
硫化ソーダ被膜は、有形物原料より相当に高い融点を有
する水硫化ソーダからなるため、その後の比較的高温脱
水においても器壁への付着や相互付着などを回避するこ
とができ、脱水処理時間を大幅に短縮し、高い回収率で
脱水することを可能にした。The present inventors, while examining various dehydration methods of sodium hydrosulfide, dehydrated at a relatively low temperature while putting a sodium hydrosulfide tangible material in a container and flowing an inert gas, It was found that the surface was gradually dehydrated and whitened, and a low water content sodium hydrosulfide coating was formed on the surface of the tangible material.
Although this whitening phenomenon varies depending on the ventilation time of the inert gas, the heating temperature, etc., when performed at atmospheric pressure and room temperature, the whitening phenomenon appears about 3 minutes after the start of the ventilation of the inert gas. It completely turned white in 40 minutes. Since the low-moisture sodium hydrosulfide coating consists of sodium hydrosulfide having a melting point considerably higher than that of the tangible material raw material, it is possible to avoid adhesion to the vessel wall or mutual adhesion even in the subsequent relatively high temperature dehydration. , The dehydration time was greatly shortened and it was possible to dehydrate with a high recovery rate.
【０００９】水硫化ソーダ有形物の白色化被膜は、原料
の水硫化ソーダ有形物の融点プラス５℃以下の温度に加
熱された不活性ガスを流して脱水するか、原料容器を原
料の水硫化ソーダの融点プラス５℃以下の温度に加熱
し、不活性ガスを流しながら脱水することにより形成す
ることができる。なお、上記の加熱手段を併用すること
も可能である。不活性ガスの流量は、水硫化ソーダ有形
物原料１００ｇ当たり毎分２ノルマルリットル以上で通
気する必要があり、好ましくは、２〜３０ノルマルリッ
トルである。The whitening film of the sodium hydrosulfide tangible substance is dehydrated by flowing an inert gas heated to a temperature not higher than the melting point of the raw material sodium hydrosulfide tangent plus 5 ° C. or by hydrolyzing the raw material container as the raw material. It can be formed by heating to a temperature not higher than the melting point of soda plus 5 ° C. and dehydrating while flowing an inert gas. It is also possible to use the above heating means together. The flow rate of the inert gas should be 2 normal liters per minute or more per 100 g of the sodium hydrosulfide tangible material, and preferably 2 to 30 normal liters.
【００１０】不活性ガスの温度が上記の融点プラス５℃
を越えたり、原料容器の温度が融点プラス５℃を越える
と、水硫化ソーダ有形物が溶融する恐れがあり、不活性
ガスの流量が毎分２ノルマルリットル未満では溶融防止
効果が少なくなり、溶融する恐れがある。また、処理時
間も長くなる。水硫化ソーダ有形物の白色化被膜を形成
するための処理時間は、３０〜１７０分、好ましくは４
０〜１２０分である。３０分より短いと完全に白色化さ
せることができず、減圧加熱脱水工程において有形物が
溶融する恐れがあり、また、１７０分を越える脱水は、
全体の脱水時間が長くなるので好ましくない。また、不
活性ガスの相対湿度（以下、水分という）は５０％以下
のものを使用する必要がある。５０％を越えると、処理
時間が長くなるので好ましくない。このように、不活性
ガス流中で水硫化ソーダ有形物を処理するので、水硫化
ソーダが空気と接触して変質することもなく、短時間で
白色化被膜を形成することができる。The temperature of the inert gas is the above melting point plus 5 ° C.
If the temperature of the raw material container exceeds the melting point plus 5 ° C, the tangible substance of sodium hydrosulfide may be melted. If the flow rate of the inert gas is less than 2 normal liters per minute, the melting prevention effect is reduced and the melting There is a risk of Also, the processing time becomes long. The processing time for forming the whitening film of the sodium hydrosulfide tangible material is 30 to 170 minutes, preferably 4 minutes.
It is 0 to 120 minutes. If it is shorter than 30 minutes, it cannot be completely whitened, and a tangible substance may melt in the dehydration process under reduced pressure, and dehydration for more than 170 minutes is
It is not preferable because the total dehydration time becomes long. Further, it is necessary to use an inert gas having a relative humidity (hereinafter referred to as water) of 50% or less. When it exceeds 50%, the processing time becomes long, which is not preferable. In this way, since the sodium hydrosulfide tangible material is treated in the inert gas flow, the whitening film can be formed in a short time without the sodium hydrosulfide coming into contact with air and being deteriorated.
【００１１】低水分の白色化被膜を備えた水硫化ソーダ
有形物は、器壁への付着や相互付着を回避し、その後の
減圧加熱脱水を極めて簡単に行うことを可能にした。な
お、この減圧加熱脱水工程における圧力は、１５トール
以下、特に１０トール以下が好ましい。１５トールを越
えると、一部に溶融付着現象がみられる。また、内容物
温度（以下、内温という）と容器の温度（以下、外温と
いう）との差を１３０℃以内、好ましくは２０〜１２０
℃の範囲で加熱脱水することが好ましい。内外温度差が
１３０℃を上回ると有形物の一部に溶融付着現象が現れ
る。The tangible substance of sodium hydrosulfide provided with a low-moisture whitening coating makes it possible to avoid adhesion to the vessel wall and mutual adhesion, and to carry out dehydration under reduced pressure heating very easily. The pressure in this reduced pressure heating dehydration step is preferably 15 Torr or less, particularly preferably 10 Torr or less. When it exceeds 15 Torr, a part of melt adhesion phenomenon is observed. Further, the difference between the content temperature (hereinafter, referred to as internal temperature) and the temperature of the container (hereinafter, referred to as external temperature) is 130 ° C or less, preferably 20 to 120.
It is preferable to heat dehydration in the range of ° C. When the temperature difference between the inside and the outside exceeds 130 ° C., a phenomenon of melt adhesion appears in a part of the tangible material.
【００１２】[0012]
【実施例】以下、本発明を実施例により説明するが、本
発明はこれらにより制限されるものではない。
（実施例１）市販のフレーク状水硫化ソーダ（約１〜２
ｃｍ2 で厚さが約１．５ｍｍ、全水硫化ソーダ分７２．
３重量％、融点５２℃）２００ｇを５００ミリリットル
のロータリーエバポレーターに入れ、内容物を攪拌しな
がら５５℃に加熱した窒素ガスを該ロータリーエバポレ
ーターの底部から毎分８ノルマルリットルで流し始めた
ところ、１５分後白色化が始まり、１１０分後に全体が
完全に白色化したので、窒素ガスの導入を停止した。こ
の時の内温は３５℃であった。次いで、該ロータリーエ
バポレーターを真空ポンプに接続し、１０トールまで減
圧した後、攪拌しながら１２０℃の恒温槽に浸し、その
後、上記の温度を保持しながら２時間３０分間脱水を行
った。その結果、全水硫化ソーダ分９８．４重量％、水
分０．２重量％のフレーク状水硫化ソーダを１３８ｇ回
収することができ、回収率は９４％であった。EXAMPLES The present invention will be described below with reference to examples, but the present invention is not limited thereto. (Example 1) Commercially available flaky sodium hydrosulfide (about 1-2)
a thickness of about 1.5mm in cm 2, total sodium hydrosulfide content 72.
(3 wt%, melting point 52 ° C.) 200 g was put into a 500 ml rotary evaporator, and nitrogen gas heated to 55 ° C. was stirred while stirring the contents, and when 8 normal liters per minute began to flow from the bottom of the rotary evaporator, 15 Whitening started after a minute, and after 110 minutes, the whole turned completely white, so the introduction of nitrogen gas was stopped. The internal temperature at this time was 35 ° C. Next, the rotary evaporator was connected to a vacuum pump, the pressure was reduced to 10 Torr, the mixture was immersed in a constant temperature bath at 120 ° C. with stirring, and then dehydration was performed for 2 hours and 30 minutes while maintaining the above temperature. As a result, 138 g of flaky sodium hydrosulfide having a total sodium hydrosulfide content of 98.4% by weight and a water content of 0.2% by weight could be recovered, and the recovery rate was 94%.
【００１３】（実施例２）実施例１の市販のフレーク状
水硫化ソーダ有形物２００ｇを５００ミリリットルのロ
ータリーエバポレーターに入れ、内容物を攪拌しながら
該ロータリーエバポレーターを５４℃の恒温槽に浸し、
室温の窒素ガスを該ロータリーエバポレーターの底部か
ら毎分８ノルマルリットルで流し始めたところ、２５分
後白色化が始まり、６０分後に全体が完全に白色化した
ので、窒素ガスの導入を停止した。この時の内温は４４
℃であった。次いで、実施例１と同様にして減圧加熱脱
水したところ、全水硫化ソーダ分９８．３重量％、水分
０．３重量％のフレーク状水硫化ソーダを１３７ｇ回収
することができ、回収率は９３％であった。(Example 2) 200 g of the commercially available flaky sodium hydrosulfide tangible material of Example 1 was put into a 500 ml rotary evaporator, and the rotary evaporator was immersed in a thermostat bath at 54 ° C while stirring the contents.
When nitrogen gas at room temperature was started to flow from the bottom of the rotary evaporator at a rate of 8 normal liters per minute, whitening started after 25 minutes, and after 60 minutes the entire whitening was complete, so the introduction of nitrogen gas was stopped. The internal temperature at this time is 44
It was ℃. Then, when dehydration under reduced pressure was carried out in the same manner as in Example 1, 137 g of flaky sodium hydrosulfide having a total sodium hydrosulfide content of 98.3% by weight and a water content of 0.3% by weight could be recovered, and the recovery rate was 93. %Met.
【００１４】（実施例３）実施例１において、窒素ガス
の供給量を毎分５ノルマルリットルに変更した以外は、
実施例１と同様にしてフレーク状水硫化ソーダ有形物の
脱水を行ったところ、全水硫化ソーダ分９８．２重量
％、水分０．４重量％のフレーク状水硫化ソーダを１３
７ｇ回収することができ、回収率は９３％であった。(Example 3) In Example 1, except that the supply rate of nitrogen gas was changed to 5 normal liters per minute.
When the flaky sodium hydrosulfide tangible material was dehydrated in the same manner as in Example 1, 13 flakes of sodium hydrosulfide having a total sodium hydrosulfide content of 98.2% by weight and a water content of 0.4% by weight were obtained.
It was possible to recover 7 g, and the recovery rate was 93%.
【００１５】（実施例４）実施例１において、フレーク
状水硫化ソーダの代わりに、水硫化ソーダ濃縮物の冷却
固化物を３〜５ｍｍ径に粉砕した水硫化ソーダ粉砕物
（全水硫化ソーダ分６７．３重量％、融点４９℃）をロ
ータリーエバポレーターに入れ、内容物を攪拌しながら
該ロータリーエバポレーターを３５℃の恒温槽に浸し、
３５℃に加熱した窒素ガスを毎分４ノルマルリットルで
流し始めてから、２５分後に白色化が始まり、１１０分
後に全体が完全に白色化したので、窒素ガスの導入を停
止した。この時の内温は３４℃であった。次いで、実施
例１と同様の方法で８トールまで減圧し、恒温槽の温度
を１３０℃まで急速に昇温し、その温度を保持しながら
３時間５０分間脱水を行った。その結果、全水硫化ソー
ダ分９８．６重量％、水分０．１重量％の水硫化ソーダ
粉砕物を１２９ｇ回収することができ、回収率は９４％
であった。(Example 4) In Example 1, instead of the flaky sodium hydrosulfide, a cooled solidified product of the sodium hydrosulfide concentrate was crushed to a diameter of 3 to 5 mm. 67.3% by weight, melting point 49 ° C.) was placed in a rotary evaporator, and while the contents were stirred, the rotary evaporator was immersed in a constant temperature bath at 35 ° C.,
Nitrogen gas heated to 35 ° C. was started to flow at 4 normal liters per minute, whitening started 25 minutes later, and after 110 minutes, the whole was completely whitened, so the introduction of nitrogen gas was stopped. The internal temperature at this time was 34 ° C. Then, the pressure was reduced to 8 Torr in the same manner as in Example 1, the temperature of the constant temperature bath was rapidly raised to 130 ° C., and dehydration was performed for 3 hours and 50 minutes while maintaining the temperature. As a result, 129 g of a sodium hydrosulfide pulverized product having a total sodium hydrosulfide content of 98.6% by weight and a water content of 0.1% by weight could be recovered, and the recovery rate was 94%.
Met.
【００１６】（比較例１）実施例１において、窒素ガス
の温度を５５℃から６５℃に変更した以外は、実施例１
と同様にしてフレーク状水硫化ソーダ有形物の脱水を行
ったところ、窒素ガス通気後１０分で溶融が始まった。Comparative Example 1 Example 1 is the same as Example 1 except that the temperature of nitrogen gas is changed from 55 ° C. to 65 ° C.
When the flaky sodium hydrosulfide tangible material was dehydrated in the same manner as above, melting started 10 minutes after aeration with nitrogen gas.
【００１７】（比較例２）実施例２において、恒温槽の
温度を５４℃から６０℃に変更した以外は、実施例２と
同様にしてフレーク状水硫化ソーダ有形物の脱水を行っ
たところ、窒素ガス通気後１０分で溶融が始まった。(Comparative Example 2) In Example 2, the flaky sodium hydrosulfide tangible product was dehydrated in the same manner as in Example 2 except that the temperature of the constant temperature bath was changed from 54 ° C to 60 ° C. Melting started 10 minutes after aeration with nitrogen gas.
【００１８】（比較例３）実施例１において、減圧加熱
脱水における圧力を２０トールにした以外は実施例１と
同様にして脱水を行ったところ、減圧加熱脱水を開始し
た後１５分後にフレークの付着現象が始まり、時間とと
もに付着が激しくなり、３５分後には内部が全く見えな
くなった。(Comparative Example 3) Dehydration was carried out in the same manner as in Example 1 except that the pressure in the reduced pressure heating dehydration was set to 20 Torr. Flake was formed 15 minutes after the reduced pressure heating dehydration was started. The adhesion phenomenon started, and the adhesion became severe with time, and after 35 minutes, the inside became completely invisible.
【００１９】（比較例４）実施例２において、窒素ガス
の供給量を毎分３ノルマルリットルに変更した以外は実
施例２と同様にして脱水を行ったところ、窒素ガスを流
し始めてから４０分後に溶融が始まった。(Comparative Example 4) Dehydration was carried out in the same manner as in Example 2 except that the supply amount of nitrogen gas was changed to 3 normal liters per minute in Example 2, and 40 minutes after starting the flow of nitrogen gas. Melting started later.
【００２０】[0020]
【発明の効果】本発明は、上記の構成を採用することに
より、水硫化ソーダを変質させることなく、短時間で高
濃度の水硫化ソーダ有形物を高い収率で得ることができ
るようになった。また、脱水処理中に水硫化ソーダ有形
物が器壁に付着したり、有形物相互に付着することもな
く、脱水処理を極めて簡単に行うことができるようにな
った。そして、かかる高濃度の水硫化ソーダは、水分を
嫌う分野特に有機化学反応への使用を可能にし、使用範
囲の拡大に大きく寄与するものである。According to the present invention, by adopting the above-mentioned constitution, it becomes possible to obtain a high-concentration sodium hydrosulfide tangible substance in a high yield in a short time without deteriorating sodium hydrosulfide. It was In addition, the sodium hydrosulfide tangible substance does not adhere to the vessel wall during the dehydration treatment, nor does the tangible substance adhere to each other, so that the dehydration treatment can be performed very easily. Further, such a high-concentration sodium hydrosulfide makes it possible to use it in fields where moisture is disliked, particularly in organic chemical reactions, and greatly contributes to the expansion of the range of use.
フロントページの続き (72)発明者 今井 伸吾 岡山県玉野市玉原１丁目15番10号 (56)参考文献 特公 昭38−3652（ＪＰ，Ｂ１) 特公 昭46−3247（ＪＰ，Ｂ１) (58)調査した分野(Int.Cl.7，ＤＢ名) C01B 17/00 - 17/98 Front page continuation (72) Inventor Shingo Imai 1-15-10 Tambara, Tamano-shi, Okayama (56) References Japanese Patent Publication No. 38-3652 (JP, B1) Japanese Patent Publication No. 46-3247 (JP, B1) (JP) 58) Fields investigated (Int.Cl. 7 , DB name) C01B 17/00-17/98
Claims (3)
する水硫化ソーダ有形物を脱水する方法において、水硫
化ソーダ有形物に不活性ガスを流して有形物の表面を脱
水した後、減圧下で加熱脱水することを特徴とする水硫
化ソーダ有形物の脱水方法。1. A method for dehydrating a sodium hydrosulfide tangible material containing 65% by weight or more of total sodium hydrosulfide, wherein an inert gas is passed through the sodium hydrosulfide tangible material to dehydrate the surface of the tangible material, and then the pressure is reduced. A method for dehydrating tangible material of sodium hydrosulfide, characterized by performing dehydration under heat.
下の温度に加熱された不活性ガスを、該原料１００ｇ当
たり毎分２ノルマルリットル以上の流量で流して有形物
の表面を脱水した後、１５トール以下の減圧下で加熱脱
水することを特徴とする請求項１記載の水硫化ソーダ有
形物の脱水方法。2. After dehydrating the surface of a tangible material by flowing an inert gas heated to a temperature not higher than the melting point of sodium hydrosulfide as a raw material plus 5 ° C. at a rate of 2 normal liters per minute or more per 100 g of the raw material. The method for dehydrating tangible substance of sodium hydrosulfide according to claim 1, wherein the dehydration is carried out by heating under a reduced pressure of 15 torr or less.
毎分２ノルマルリットル以上の流量で不活性ガスを流し
ながら、該原料を収容する容器を原料の水硫化ソーダの
融点プラス５℃以下の温度に加熱して有形物の表面を脱
水した後、１５トール以下の減圧下で加熱脱水すること
を特徴とする請求項１記載の水硫化ソーダ有形物の脱水
方法。3. A container containing the raw material of sodium hydrosulfide is heated to a temperature not higher than the melting point of the raw material sodium hydrosulfide plus 5 ° C. while flowing an inert gas at a flow rate of 2 normal liters per minute or more per 100 g of the sodium hydrosulfide tangible material. The method for dehydrating a tangible substance of sodium hydrosulfide according to claim 1, wherein after the surface of the tangible substance is heated to be dehydrated, it is heated and dehydrated under a reduced pressure of 15 Torr or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08603093A JP3408575B2 (en) | 1993-04-13 | 1993-04-13 | Dehydration method of tangible sodium hydrosulfide with inert gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08603093A JP3408575B2 (en) | 1993-04-13 | 1993-04-13 | Dehydration method of tangible sodium hydrosulfide with inert gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06298502A JPH06298502A (en) | 1994-10-25 |
| JP3408575B2 true JP3408575B2 (en) | 2003-05-19 |
Family
ID=13875267
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP08603093A Expired - Lifetime JP3408575B2 (en) | 1993-04-13 | 1993-04-13 | Dehydration method of tangible sodium hydrosulfide with inert gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3408575B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19755760A1 (en) * | 1997-12-16 | 1999-06-24 | Degussa | Process for the preparation of anhydrous sodium sulfide |
| US6503474B1 (en) | 1997-12-16 | 2003-01-07 | Degussa Ag | Process for the preparation of anhydrous sodium sulfide |
-
1993
- 1993-04-13 JP JP08603093A patent/JP3408575B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06298502A (en) | 1994-10-25 |
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