JP3017714B2 - Method for producing aqueous solution of hydrazinium carbazate salt - Google Patents
Method for producing aqueous solution of hydrazinium carbazate saltInfo
- Publication number
- JP3017714B2 JP3017714B2 JP10156146A JP15614698A JP3017714B2 JP 3017714 B2 JP3017714 B2 JP 3017714B2 JP 10156146 A JP10156146 A JP 10156146A JP 15614698 A JP15614698 A JP 15614698A JP 3017714 B2 JP3017714 B2 JP 3017714B2
- Authority
- JP
- Japan
- Prior art keywords
- aqueous solution
- hydrazinium
- hydrazine hydrate
- salt
- carbazinate
- 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 - Fee Related
Links
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明はカルバジン酸ヒドラ
ジニウム塩水溶液の製造方法に関する。[0001] The present invention relates to a method for producing an aqueous solution of hydrazinium carbazinate.
【０００２】[0002]
【従来の技術】カルバジン酸ヒドラジニウム塩（ＮＨ2
ＮＨＣＯ2 - +Ｎ2Ｈ5）は、脱酸素剤、スライムコントロ
ール剤、還元剤、エッチング剤等の分野において有用な
化合物である。2. Description of the Related Art Hydrazinium carbazinate (NH 2)
NHCO 2 − + N 2 H 5 ) is a compound useful in the fields of oxygen scavengers, slime control agents, reducing agents, etching agents and the like.
【０００３】従来、カルバジン酸ヒドラジニウム塩の製
造方法としては、（１）炭酸ヒドラジンを１４０℃程度
で加熱濃縮して得る方法、（２）カルバジン酸を加熱分
解して得る方法等が知られている。Heretofore, as a method for producing hydrazinium carbazinate, there are known a method of (1) obtaining hydrazine carbonate by heating and concentrating it at about 140 ° C., and a method of (2) obtaining carbazine acid by thermal decomposition. .
【０００４】これらの方法は、それ自体多大なエネルギ
ーを必要とする方法であるのみならず、更に、カルバジ
ン酸ヒドラジニウム塩を脱酸素剤やスライムコントロー
ル剤として用いる際には得られた結晶物を水に溶解させ
水溶液として調製する工程を必要とし、従って、製造工
程が極めて煩雑なものであった。[0004] These methods not only require a large amount of energy per se, but furthermore, when the hydrazinium carbazinate is used as an oxygen scavenger or a slime control agent, the obtained crystals are treated with water. And a step of dissolving the same in an aqueous solution was required, and the production process was extremely complicated.
【０００５】[0005]
【発明が解決しようとする課題】本発明は、結晶物を経
由しない簡便なカルバジン酸ヒドラジニウム塩水溶液の
製造方法を提供することを課題とする。SUMMARY OF THE INVENTION An object of the present invention is to provide a simple method for producing a hydrazinium carbazate aqueous solution without passing through a crystal.
【０００６】[0006]
【課題を解決するための手段】かかる課題を解決するた
め、本発明は以下の技術的手段を講じる。即ち、本発明
は１モルのヒドラジンヒドラート（Ｎ2Ｈ4・Ｈ2Ｏ）又
はその水溶液（以下、単にヒドラジンヒドラートという
ことがある）と、約１／２モルの二酸化炭素とを反応さ
せることを特徴とするカルバジン酸ヒドラジニウム塩水
溶液の製造方法に係る。In order to solve such a problem, the present invention takes the following technical means. That is, the present invention reacts 1 mol of hydrazine hydrate (N 2 H 4 .H 2 O) or an aqueous solution thereof (hereinafter, sometimes simply referred to as hydrazine hydrate) with about 1/2 mol of carbon dioxide. The present invention relates to a method for producing a hydrazinium carbazinate aqueous solution, characterized by the above-mentioned.
【０００７】本発明において、ヒドラジンヒドラートの
濃度としては、５〜１００重量％程度とするのがよく、
好ましくは６０〜９０重量％とするのがよい。濃度６０
重量％以上のヒドラジンヒドラートを用いることで生産
効率を上げることができ、濃度９０重量％以下のヒドラ
ジンヒドラートを用いることで二酸化炭素との反応効率
を上げることができる。In the present invention, the concentration of hydrazine hydrate is preferably about 5 to 100% by weight.
Preferably, the content is 60 to 90% by weight. Concentration 60
The production efficiency can be increased by using hydrazine hydrate in an amount of not less than 90% by weight, and the reaction efficiency with carbon dioxide can be increased by using hydrazine hydrate having a concentration of not more than 90% by weight.
【０００８】二酸化炭素の使用量としては、ヒドラジン
ヒドラート１モルに対し約１／２モル相当量とするのが
好ましい。二酸化炭素の使用量が多すぎると、目的とす
る水溶液中のカルバジン酸ヒドラジニウム塩の純度が低
下し、一方、二酸化炭素使用量が少なすぎると、未反応
のヒドラジンヒドラートが多く残存するため好ましくな
いからである。[0008] The amount of carbon dioxide used is preferably about 1/2 mole equivalent to 1 mole of hydrazine hydrate. If the amount of carbon dioxide used is too large, the purity of the carbazinate hydrazinium salt in the intended aqueous solution decreases, while if the amount of carbon dioxide used is too small, a large amount of unreacted hydrazine hydrate remains unpreferably. Because.
【０００９】ヒドラジンヒドラートと二酸化炭素との反
応は、通常、ヒドラジンヒドラート中に炭酸ガスを吹き
込むことにより進行させることができる。該反応は、好
ましくは攪拌下に行うのがよい。[0009] The reaction between hydrazine hydrate and carbon dioxide can usually be advanced by blowing carbon dioxide gas into hydrazine hydrate. The reaction is preferably carried out with stirring.
【００１０】また、９０重量％を超える高濃度のヒドラ
ジンヒドラートを使用する場合は、反応液の粘度が高く
なるため炭酸ガスの導入が若干困難となり反応効率が低
下する虞があるため、そのような場合には強い攪拌下に
反応を進行させるのが好ましい。When hydrazine hydrate having a high concentration of more than 90% by weight is used, the viscosity of the reaction solution becomes high, so that the introduction of carbon dioxide gas becomes slightly difficult, and the reaction efficiency may be reduced. In such a case, the reaction is preferably allowed to proceed under strong stirring.
【００１１】反応は、通常、０〜５０℃程度、好ましく
は５〜３０℃程度で進行させることができる。反応は、
通常、炭酸ガス導入後、１時間程度で完了する。[0011] The reaction can be usually carried out at about 0 to 50 ° C, preferably about 5 to 30 ° C. The reaction is
Usually, it is completed in about one hour after the introduction of carbon dioxide gas.
【００１２】本発明の製造方法により得られるカルバジ
ン酸ヒドラジニウム塩の水溶液はそのまま使用すること
ができ、また所定量の水を添加し、又は減圧若くは加熱
濃縮することにより容易に任意の濃度に調整することが
できる。The aqueous solution of hydrazinium carbazinate obtained by the production method of the present invention can be used as it is, and can be easily adjusted to an arbitrary concentration by adding a predetermined amount of water, or by concentrating under reduced pressure or by heating. can do.
【００１３】[0013]
【実施例】以下にカルバジン酸ヒドラジニウム塩の水溶
液の製造に関して種々の実施例を挙げ、本発明を更に詳
細に説明する。EXAMPLES The present invention will be described in more detail with reference to various examples relating to the production of an aqueous solution of hydrazinium carbazinate.
【００１４】＜実施例１＞攪拌機、温度計及びガス導入
管を備えた２００ｍｌ容の四つ口ナス型フラスコに、８
０重量％のヒドラジンヒドラート水溶液１００ｇ（１．
６モル）を仕込んだ。Example 1 A 200 ml four-necked eggplant type flask equipped with a stirrer, thermometer and gas inlet tube was charged with 8
100 g of a 0% by weight aqueous solution of hydrazine hydrate (1.
6 mol).
【００１５】攪拌下、２０℃以下を保つように冷却しな
がら、ガス導入管より炭酸ガス３５．２ｇ（０．８モ
ル）を１時間かけて導入した。While stirring and cooling so as to keep the temperature at 20 ° C. or lower, 35.2 g (0.8 mol) of carbon dioxide gas was introduced from the gas inlet tube over 1 hour.
【００１６】その後、１時間攪拌した後、反応を停止
し、目的とするカルバジン酸ヒドラジニウム塩の６４重
量％の水溶液１３５．２ｇ（収率１００％）を得た。After stirring for 1 hour, the reaction was stopped to obtain 135.2 g (yield: 100%) of a 64% by weight aqueous solution of the desired hydrazinium carbazinate.
【００１７】得られた水溶液を減圧（１ｍｍＨｇ）・低
温（５０℃以下）の条件下にて水を留去し得られた結晶
について、還元性滴定、融点及びＩＲスペクトルを測定
したところ、従来法で得られたカルバジン酸ヒドラジニ
ウム塩の評品と完全に一致した。The resulting aqueous solution was distilled under reduced pressure (1 mmHg) and low temperature (50 ° C. or less). The crystals obtained were measured for reductive titration, melting point and IR spectrum. Completely matched the evaluation of the hydrazinium carbazinate obtained in the above.
【００１８】＜実施例２＞攪拌機、温度計及びガス導入
管を備えた２００ｍｌ容の四つ口ナス型フラスコに、１
００重量％のヒドラジンヒドラート水溶液１００ｇ
（２．０モル）を仕込んだ。Example 2 A 200 ml four-necked eggplant type flask equipped with a stirrer, thermometer and gas inlet tube was charged with 1
100 g of a 00% by weight aqueous solution of hydrazine hydrate
(2.0 mol).
【００１９】攪拌下、２０℃以下を保つように冷却しな
がら、ガス導入管より液化炭酸ガス４４ｇ（１．０モ
ル）を２時間かけて導入した。While stirring and cooling so as to maintain the temperature at 20 ° C. or lower, 44 g (1.0 mol) of liquefied carbon dioxide gas was introduced from a gas introduction tube over 2 hours.
【００２０】その後、１時間攪拌した後、反応を停止
し、目的とするカルバジン酸ヒドラジニウム塩の７５重
量％の水溶液１４４ｇ（収率１００％）を得た。After stirring for 1 hour, the reaction was stopped to obtain 144 g (100% yield) of a 75% by weight aqueous solution of the desired hydrazinium carbazinate.
【００２１】＜実施例３＞攪拌機、温度計及びガス導入
管を備えた２００ｍｌ容の四つ口ナス型フラスコに、８
０重量％のヒドラジンヒドラート水溶液１００ｇ（１．
６モル）を仕込んだ。Example 3 A 200 ml four-necked eggplant type flask equipped with a stirrer, thermometer and gas inlet tube was charged with 8
100 g of a 0% by weight aqueous solution of hydrazine hydrate (1.
6 mol).
【００２２】攪拌下、２０℃以下を保つように冷却しな
がら、ガス導入管よりドライアイス３５．２ｇ（０．８
モル）を１時間かけて徐々に添加した。35.2 g (0.8%) of dry ice was introduced from the gas inlet tube while cooling to keep the temperature at 20 ° C. or lower under stirring.
Mol) was added slowly over 1 hour.
【００２３】その後、１時間攪拌した後、反応を停止
し、目的とするカルバジン酸ヒドラジニウム塩の６４重
量％の水溶液１３５．２ｇ（収率１００％）を得た。After stirring for 1 hour, the reaction was stopped to obtain 135.2 g (yield: 100%) of a 64% by weight aqueous solution of the desired hydrazinium carbazinate.
【００２４】[0024]
【発明の効果】本発明の方法によれば、極めて簡便な方
法によって任意の濃度のカルバジン酸ヒドラジニウム塩
の水溶液を高収率で製造することができる。According to the method of the present invention, an aqueous solution of hydrazinium carbazate at an arbitrary concentration can be produced in a high yield by a very simple method.
フロントページの続き (56)参考文献 特開 平８−134038（ＪＰ，Ａ) Ｊ．Ｉｎｏｒｇ．Ｎｕｃｌ．Ｃｈｅ ｍ．，（1979）41（７）Ｐ．953−955 Ｐｒｏ．Ｉｎｄｉａｎ Ａｃａｄ．Ｓ ｃｉ．（Ｃｈｅｍ．Ｓｃｉ．）, （1985）95（４）Ｐ．345−356 (58)調査した分野(Int.Cl.7，ＤＢ名) C07C 281/02 ＣＡＰＬＵＳ（ＳＴＮ)Continuation of front page (56) References JP-A-8-134038 (JP, A) Inorg. Nucl. Chem. , (1979) 41 (7) P. 953-955 Pro. Indian Acad. S ci. (Chem. Sci.), (1985) 95 (4) p. 345-356 (58) Field surveyed (Int. Cl. 7 , DB name) C07C 281/02 CAPLUS (STN)
Claims (2)
水溶液と、約１／２モルの二酸化炭素とを反応させるこ
とを特徴とするカルバジン酸ヒドラジニウム塩水溶液の
製造方法。1. A method for producing an aqueous hydrazinium carbazate salt solution, comprising reacting 1 mol of hydrazine hydrate or an aqueous solution thereof with about 1/2 mol of carbon dioxide.
６０〜９０重量％のものを用いる請求項１記載のカルバ
ジン酸ヒドラジニウム塩水溶液の製造方法。2. The concentration as an aqueous solution of hydrazine hydrate.
The method for producing an aqueous solution of a hydrazinium carbazate salt according to claim 1, wherein the aqueous solution is 60 to 90% by weight .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10156146A JP3017714B2 (en) | 1998-06-04 | 1998-06-04 | Method for producing aqueous solution of hydrazinium carbazate salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10156146A JP3017714B2 (en) | 1998-06-04 | 1998-06-04 | Method for producing aqueous solution of hydrazinium carbazate salt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11349554A JPH11349554A (en) | 1999-12-21 |
| JP3017714B2 true JP3017714B2 (en) | 2000-03-13 |
Family
ID=15621345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10156146A Expired - Fee Related JP3017714B2 (en) | 1998-06-04 | 1998-06-04 | Method for producing aqueous solution of hydrazinium carbazate salt |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3017714B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101363595B1 (en) * | 2012-03-12 | 2014-02-17 | 서강대학교산학협력단 | Products from Reactions of Hydrazine Derivatives with Carbon Dioxide |
| KR101383762B1 (en) * | 2012-03-20 | 2014-04-10 | 서강대학교산학협력단 | Carbon Dioxide Capture Sorbent and Method for Carbon Dioxide Capture |
-
1998
- 1998-06-04 JP JP10156146A patent/JP3017714B2/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| Ｊ．Ｉｎｏｒｇ．Ｎｕｃｌ．Ｃｈｅｍ．，（１９７９）４１（７）Ｐ．９５３−９５５ |
| Ｐｒｏ．Ｉｎｄｉａｎ Ａｃａｄ．Ｓｃｉ．（Ｃｈｅｍ．Ｓｃｉ．），（１９８５）９５（４）Ｐ．３４５−３５６ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH11349554A (en) | 1999-12-21 |
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