CN1079094C - Process for preparing high-purity malononitrile - Google Patents
Process for preparing high-purity malononitrile Download PDFInfo
- Publication number
- CN1079094C CN1079094C CN98111529A CN98111529A CN1079094C CN 1079094 C CN1079094 C CN 1079094C CN 98111529 A CN98111529 A CN 98111529A CN 98111529 A CN98111529 A CN 98111529A CN 1079094 C CN1079094 C CN 1079094C
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- China
- Prior art keywords
- malononitrile
- purity
- propane dinitrile
- production method
- crude product
- 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.)
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Abstract
The present invention discloses a production method of high-purity malononitrile, which comprises: the malononitrile as a crude product is dissolved in anhydrous alcohol, cooled, crystallized and centrifugated, and then the malononitrile is treated through distillation under reduced pressure, distillation fraction collection, etc. The present invention obviously improves the product quality of the malononitrile, the quality index of the malononitrile is greater than or equal to 99.9%, the appearance is colorless, the pH value is neutral, the acidity is less than 0.1%, and the crystallization point is higher than 31.4DEG C.
Description
The present invention relates to a kind of production method of propane dinitrile.
Contain the phosphorus of a certain amount of hydrochloric acid and trace in the technical grade propane dinitrile, make its purposes be restricted, and rough propane dinitrile product to store a couple of days will chlorination rubescent, the time has been grown also polymerization can take place.
The object of the present invention is to provide a kind of production technique that rough propane dinitrile is refined into the high high-purity malononitrile of purity.
Technical solution of the present invention is:
A kind of production method of high-purity malononitrile, the difference of itself and prior art is: comprise the following steps:
With propane dinitrile crude product anhydrous alcohol solution, cooling again, crystallization, centrifugal are collected fraction through underpressure distillation then, promptly get high-purity malononitrile.
The weight proportion of propane dinitrile and dehydrated alcohol is a propane dinitrile: ethanol=1: 0.2～1.0.Underpressure distillation is collected fraction and is carried out under 90-100 ℃/6-10mmHg condition.
The present invention has adopted recrystallization to technical grade propane dinitrile crude product--rectification method, and make its quality product obtain obviously to improve, its quality index is 〉=99.9%, appearance colorless, PH neutrality, acidity＜0.1%, ctystallizing point is more than 31.4 ℃.
The invention will be further described below in conjunction with embodiment:
Embodiment 1:
A kind of production method of high-purity malononitrile comprises the following steps:
Technical grade propane dinitrile crude product is pressed propane dinitrile with dehydrated alcohol: the weight proportion dissolving of ethanol=1: 0.3, more routinely the ethyl alcohol recrystallization method cool off, crystallization, centrifugal treating, collect the fraction of 95 ℃/8mmHg then through underpressure distillation.Promptly get high-purity malononitrile, its quality index is 〉=99.9%, appearance colorless, and PH neutrality, acidity＜0.1%, ctystallizing point is more than 31.4 ℃.
Embodiment 2:
A kind of production method of high-purity malononitrile comprises the following steps:
The propane dinitrile crude product is pressed propane dinitrile with dehydrated alcohol: the weight proportion dissolving of ethanol=1: 0.6, more routinely the ethyl alcohol recrystallization method cool off, crystallization, centrifugal treating, collect the fraction of 90 ℃/9mmHg then through underpressure distillation.Promptly get high-purity malononitrile, its quality index is substantially with embodiment 1.Embodiment 3:
A kind of production method of high-purity malononitrile comprises the following steps:
Technical grade propane dinitrile crude product is pressed propane dinitrile with dehydrated alcohol: the weight proportion dissolving of ethanol=1: 0.9, more routinely the ethyl alcohol recrystallization method cool off, crystallization, centrifugal treating, collect the fraction of 100 ℃/7mmHg then through underpressure distillation.Promptly get high-purity malononitrile, its quality index is substantially with embodiment 1.
Claims (3)
1, a kind of production method of high-purity malononitrile is characterized in that: comprise the following steps:
With propane dinitrile crude product anhydrous alcohol solution, cooling again, crystallization, centrifugal are collected fraction through underpressure distillation then, promptly get high-purity malononitrile.
2, the production method of high-purity malononitrile according to claim 1 is characterized in that: the weight proportion of propane dinitrile and dehydrated alcohol is a propane dinitrile: ethanol=1: 0.2～1.0.
3, the production method of high-purity malononitrile according to claim 1 and 2 is characterized in that: underpressure distillation is collected fraction and is carried out under 90-100 ℃/6-10mmHg condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98111529A CN1079094C (en) | 1998-10-09 | 1998-10-09 | Process for preparing high-purity malononitrile |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98111529A CN1079094C (en) | 1998-10-09 | 1998-10-09 | Process for preparing high-purity malononitrile |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1250772A CN1250772A (en) | 2000-04-19 |
| CN1079094C true CN1079094C (en) | 2002-02-13 |
Family
ID=5221502
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98111529A Expired - Fee Related CN1079094C (en) | 1998-10-09 | 1998-10-09 | Process for preparing high-purity malononitrile |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1079094C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342661A (en) * | 2013-07-19 | 2013-10-09 | 中国海洋石油总公司 | Crystal purifying method of high purity butanedinitrile |
| CN107915660B (en) * | 2016-10-10 | 2021-01-01 | 惠州市宙邦化工有限公司 | Purification method of butanedinitrile |
| CN112679385B (en) * | 2020-12-31 | 2022-09-09 | 河北诚信集团有限公司 | Purification method of malononitrile |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5818347A (en) * | 1981-07-27 | 1983-02-02 | Mitsubishi Gas Chem Co Inc | Separating and purifying method of malononitrile |
-
1998
- 1998-10-09 CN CN98111529A patent/CN1079094C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5818347A (en) * | 1981-07-27 | 1983-02-02 | Mitsubishi Gas Chem Co Inc | Separating and purifying method of malononitrile |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1250772A (en) | 2000-04-19 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |