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Process for removing hydrogen cyanide from ethanedinitrile

A technology of hydrogen cyanide and ethanedinitrile, applied in chemical instruments and methods, cyanide, cyanide, etc., can solve problems such as inappropriate ethanedinitrile, and achieve the effects of simplified processing, cheap purchase, and easy preparation

Inactive Publication Date: 2011-08-10
LONZA LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, under these basic conditions, the hydrolysis of ethanedinitrile will be unavoidable, so that the method is not suitable for the purification of ethanedinitrile

Method used

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  • Process for removing hydrogen cyanide from ethanedinitrile
  • Process for removing hydrogen cyanide from ethanedinitrile
  • Process for removing hydrogen cyanide from ethanedinitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Preparation of oxalonitrile and purification with sodium glyoxylate

[0040] In a 2L stirring device (Labmax) with temperature control jacket, stirrer, reflux condenser, pH meter and two feeding systems, 25.3g of iron sulfate (Ⅲ) hydrate and 24.7g of copper sulfate (II) pentahydrate are combined The substance was dissolved in 308ml water. Within 120 min, 100 g hydrogen cyanide (100%) and 209 g hydrogen peroxide (30%) were added dropwise at 20°C.

[0041] The gas formed during the reaction has the following components: (analyzed by gas chromatography):

[0042] Oxalonitrile: 90.0%

[0043] Hydrogen cyanide: 1.00%

[0044] Water: 0.60%

[0045] Carbon dioxide: 8.40%

[0046] The resulting gas mixture was passed through a gas scrubber containing 10% sodium glyoxylate aqueous solution (prepared from sodium hydroxide aqueous solution and glyoxylic acid aqueous solution), and then passed through a gas scrubber bottle equipped with molecular sieve (3A) for drying. After thes...

Embodiment 2

[0053] Example 2: Preparation of oxalonitrile and purification with glyoxylic acid

[0054] In a 2L stirring device (Labmax) with temperature control jacket, stirrer, reflux condenser, pH meter and two feeding systems, 7.5g iron sulfate (Ⅲ) hydrate and 7.5g copper sulfate (II) pentahydrate are combined The substance was dissolved in 308ml water. Within 120 minutes, 136 g hydrogen cyanide (100%) and 288 g hydrogen peroxide (30%) were added dropwise at 20°C.

[0055] The gas formed during the reaction has the following components: (analyzed by gas chromatography):

[0056] Oxalonitrile: 90.40%

[0057] Hydrogen cyanide: 4.40%

[0058] Water: 0.58%

[0059] Carbon dioxide: 4.60%

[0060] The resulting gas mixture was passed through a gas scrubber containing a 10% glyoxylic acid aqueous solution, and then passed through a gas scrubber bottle equipped with molecular sieves for drying. After these washing and drying steps, the oxonitrile gas has the following composition (analyzed by gas ch...

Embodiment 3

[0067] Example 3: Preparation of oxonitrile and purification with cyclohexanone

[0068] In a 2L stirring device (Labmax) with temperature control jacket, stirrer, reflux condenser, pH meter and two feeding systems, 25.3g of iron sulfate (Ⅲ) hydrate and 24.7g of copper sulfate (II) pentahydrate are combined The substance was dissolved in 308ml water. Within 120 min, 100 g hydrogen cyanide (100%) and 251 g hydrogen peroxide (30%) were added dropwise at 15°C.

[0069] The gas mixture formed in the reaction was passed through a gas scrubber containing 38.3 mL of cyclohexanone and 0.5 g of sodium cyanide, followed by a reflux condenser cooled to -10°C. After these washing and drying steps, oxalonitrile was obtained in 60% yield and had the following components (analyzed by gas chromatography):

[0070] Oxalonitrile: 79.71%

[0071] Hydrogen cyanide: 0.68%

[0072] Water: —

[0073] Carbon dioxide: 19.58%

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Abstract

Process for removing hydrogen cyanide from ethanedinitrile by contacting hydrogen cyanide-containing ethanedinitrile with an organic reagent under formation of a covalent bond.

Description

Technical field [0001] The present invention relates to a method for removing hydrogen cyanide in oxonitrile. Background technique [0002] Oxalonitrile, also known as dicyanide, is a colorless and toxic gas with a sweet pungent odor and a boiling point of -21°C. Chemically, its performance is similar to halogen, so it is called pseudo halogen. Oxalonitrile is an important intermediate for the preparation of many commercial end products (such as synthetic fertilizers and nitriles). In addition, oxalonitrile can be used in the welding process because it burns with oxygen in the hottest flame (4640K) known. Other fields of application of oxonitrile are its use as a high-performance fuel, as a stabilizer in the preparation of nitrocellulose, or as a fumigant, especially in agriculture, for example to kill parasites on agricultural soils. Or used in commodity storage (WO 2005 / 037332, US 6,001,383). [0003] Oxalonitrile can be prepared in the laboratory by heating mercury(II) cyani...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C3/00
CPCC01C3/003C07C253/34C07C255/04
Inventor 保罗·汉塞尔曼埃伦·克莱格尔夫沃尔夫冈·温格
Owner LONZA LTD
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