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Method for producing tetraethyl orthocarbonate with coproduction of 5-chlorovaleronitrile

A technology of tetraethyl orthocarbonate and chlorovaleronitrile, applied in chemical instruments and methods, preparation of organic compounds, preparation of cyanide reactions, etc., can solve problems such as difficult treatment of cyanide, and achieve low toxicity of waste water and good social economy. Benefit, simple operation effect

Inactive Publication Date: 2014-05-21
GENCHEM & GENPHARM CHANGZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This technology uses five chemicals: 1) 2-(tetrahydrothymolynoic acid), 3) 4-cyano-4'-morpholine-3-one (CNAM), 6) N-2-dim ethoxyimino-1 - propane spheroid salt (NIM). These materials help improve productivity by producing 5- chlorsalicylic acid instead of making it from tetraEthanol AMP or other sources like ammonia gas. Additionally, these chemistries are less expensive compared to traditional methods such as nitrogen removal processes because they use fewer raw material resources. Overall, this method provides an efficient way to produce high purity alkali metal salts without generating harmful wastes during manufacturing process.

Problems solved by technology

The technical problem addressed in this patented technology relates to producing high purity tetrahydroorthocyclodecane monomer from dichloromalonic acid esters through chemical reactions involving specific substances like nitroimides or other compounds called catalysts.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Add 2000kg of absolute ethanol and 420kg of sodium ethoxide into a 5000-liter reactor, heat up to the reflux temperature under stirring, then drop 220kg of trichloroacetonitrile evenly within 5 to 6 hours, and react for 1 hour after the addition is complete. A large amount of white sodium chloride and sodium cyanide salts were precipitated in the feed liquid in the kettle, which was in a suspended state.

[0024] (2) Steam 1500kg of absolute ethanol under normal pressure, cool the liquid in the kettle to room temperature, add 2000kg of water, stir at room temperature to dissolve the precipitated sodium chloride and sodium cyanide, and then add 840kg of petroleum ether;

[0025] (3) After stirring for 0.5 hours, let stand and separate the phases, the upper layer is the organic phase, and the lower layer is the aqueous phase;

[0026] (4) The upper organic phase enters the rectification tower, and the petroleum ether with a distillate temperature of 60-90°C is distill...

Embodiment 2

[0032] (1) Add 1740Kg of absolute ethanol and 435Kg of sodium ethoxide into a 5000-liter reactor, heat up to the reflux temperature under stirring, then drop 220kg of trichloroacetonitrile evenly within 5 to 6 hours, and react for 1 hour after the addition is complete. A large amount of white sodium chloride and sodium cyanide salts were precipitated in the feed liquid in the kettle, which was in a suspended state.

[0033] (2) Steam 1218kg of absolute ethanol under normal pressure, cool the liquid in the kettle to room temperature, add 1740kg of water, stir at room temperature to dissolve the precipitated sodium chloride and sodium cyanide, then add 870kg of petroleum ether,

[0034] (3) After stirring for 45 minutes, let stand and separate the phases, the upper layer is the organic phase, and the lower layer is the aqueous phase;

[0035] (4) The upper organic phase enters the rectification tower, distills petroleum ether with a distillate temperature of 60-90°C under normal...

Embodiment 3

[0040] (1) Add 2486.5Kg of absolute ethanol and 497.3Kg of sodium ethoxide into a 5000-liter reactor, heat up to reflux temperature under stirring, then drop 220Kg of trichloroacetonitrile evenly within 5 to 6 hours, and react for 1 hour after the addition is complete. At this time, a large amount of white sodium chloride and sodium cyanide salts were precipitated in the feed liquid in the kettle, and were in a suspended state.

[0041] (2) Steam 1741kg of absolute ethanol under normal pressure, cool the liquid in the kettle to room temperature, add 2486.5kg of water, stir at room temperature to dissolve the precipitated sodium chloride and sodium cyanide, and then add 994.6kg of petroleum ether.

[0042] (3) After stirring for 1 hour, stand still and separate the phases, the upper layer is the organic phase, and the lower layer is the aqueous phase;

[0043] (4) The upper organic phase enters the rectification tower, and distills petroleum ether at a temperature of 60-90°C un...

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Abstract

The invention relates to the fine chemical engineering field and in particular relates to method for producing a medical intermediate tetraethyl orthocarbonate with coproduction of 5-chlorovaleronitrile. The method comprises the steps of reacting trichloroacetonitrile with sodium ethoxide in absolute ethyl alcohol to obtain the ethyl alcohol solution of the tetraethyl orthocarbonate, and separating out a solid salt sodium chloride and sodium cyanide, evaporating out 70%-75% of absolute ethyl alcohol and then adding water, stirring and standing to split phases, introducing the organic phase to a rectifying tower for rectification, pouring the water phase into a reaction device, and adding 1,4-dichlorobutane and a catalyst for reacting. The method has the advantages that the 5-chlorovaleronitrile is produced while the tetraethyl orthocarbonate is produced, more than 99% of sodium cyanide is utilized and consumed, and as a result, the production efficiency is improved, and the technical problem that the cyanides in the wastewater are difficult to dispose when the tetraethyl orthocarbonate is produced is solved successfully; the method is simple to operate; after being treated, the wastewater is low in toxicity, so that the cost and danger of wastewater treatment are greatly reduced; as a result, the method is especially applicable to industrial production and has tremendous social and economic benefits.

Description

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Claims

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Application Information

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Owner GENCHEM & GENPHARM CHANGZHOU CO LTD
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