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Process for producing alkyl nitrite

The technology of an alkyl nitrite and process is applied in the field of preparing the alkyl nitrite, can solve the problems of environmental pollution, low yield of the alkyl nitrite and the like, and achieves the effects of improving the reaction rate and improving the yield

Active Publication Date: 2013-02-13
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0020] The purpose of the present invention is to provide a kind of method for preparing alkyl nitrite for the above appeal to the improvement of synthetic alkyl nitrite process, this technology prepares alkyl nitrite by nitrogen oxide and alkyl alcohol, fully utilizes The by-product nitric acid generated in the reaction solves the environmental pollution problems caused by the low yield of alkyl nitrite caused by the generation of nitric acid in the reaction of nitrogen oxides and the discharge of waste water containing nitric acid

Method used

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  • Process for producing alkyl nitrite

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Experimental program
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Effect test

Embodiment 1

[0047] Contains N 2 and NO mixed gas (the total gas flow rate is 284 mL / min, where N 2 volume fraction is 77.8%, NO volume fraction is 22.2%) enters the reactor I that is equipped with 50% nitric acid solution (weight percentage), the reaction pressure of reactor I is 0.1 MPa, and reaction temperature is 30 o C, the contact time of mixed gas and nitric acid solution in reactor I is 1 second. The tail gas after the reaction enters the reactor II through the pipeline, and the O 2 reaction, and keep the reaction O 2 The volume ratio to NO is 0.5. The nitrogen oxides generated after the reaction in the reactor II enter the reactor III through the pipeline, and the reactor III is equipped with an excessive amount of pure ethanol solution. After the nitrogen oxides react with the ethanol solution, the generated ethyl nitrite is discharged from the pipeline Collection, wherein the generation rate of ethyl nitrite is 103.5 mmol / h.

[0048] The nitric acid solution after the react...

Embodiment 2

[0050] The O introduced into the reactor II 2 The amount is reduced to 0, i.e. the O in the reactor II is maintained in the reaction 2 The volume ratio to NO is 0, and other conditions are the same as those in Embodiment 1. The formation rate of ethyl nitrite was 44.1 mmol / h.

Embodiment 3

[0052] Contains N 2 and NO mixed gas (the total gas flow rate is 284 mL / min, where N 2 The volume fraction is 77.8%, the NO volume fraction is 22.2%) enters the reactor I that is equipped with 15% nitric acid solution (weight percentage), the reaction pressure of reactor I is 0.5 MPa, and reaction temperature is 90 o C, the contact time of mixed gas and nitric acid solution in reactor I is 50 seconds. The tail gas after the reaction enters the reactor II through the pipeline, and the O 2 reaction, and keep the reaction O 2 The volume ratio to NO is 0.2. The nitrogen oxide enters the reactor III through the pipeline, and the excess pure ethanol solution is installed in the reactor III. After the nitrogen oxide reacts with the ethanol solution, the generated ethyl nitrite is discharged and collected through the pipeline, and the generation of ethyl nitrite The rate was 94.5 mmol / h.

[0053] The nitric acid solution after the reaction in the reactor I and the solution after ...

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Abstract

The invention discloses a process for producing alkyl nitrite. The process comprises the following step of: based on a nitric oxide and alkyl alcohol as raw materials, preparing alkyl nitrite by recycling by-products formed in the reaction process of the nitric oxide (NOx) and alcoholic solution. The process is applicable under the condition that O2 is involved or not involved, and before the nitric oxide and O2 are in contact reaction, a molar ratio of O2 to NO in the nitric oxide is not more than 0.5 under the condition that O2 is involved. According to the process, nitrogen is basically not consumed, the yield of alkyl nitrite is improved, and the reaction rate is improved; generated nitric acid is concentrated and can be recycled, the solvent is not consumed, wastewater is not generated, and the effects of recycling industrial effluent gas, saving energy, reducing emission and changing wastes into valuable materials are achieved; and meanwhile, the process is applicable under the condition that O2 is involved or not involved.

Description

technical field [0001] The present invention relates to a kind of method for preparing alkyl nitrite, relate to a kind of more specifically in the presence of O 2 or without O 2 In the case of participating in the reaction, nitrogen oxides and alkyl alcohols are used as raw materials, and nitrogen oxides (NO x ) and the by-product nitric acid formed in the reaction process of alcohol solution to prepare the method of alkyl nitrite. Background technique [0002] Alkyl nitrite (alkyl nitrite) has many uses. It can be used as a stabilizer for unsaturated organic compounds, an additive for motor oil, and a reagent for nitrosation and diazotization. At the same time, alkyl nitrite It can be used to produce alkyl oxalate. [0003] At present, the synthesis of alkyl nitrite is mostly based on nitrogen oxides (such as NO, NO 2 , N 2 o 3 , N 2 o 4 ), O 2 Synthesized with alkanol as raw material, alkanol is ethanol as an example, according to literature reports ("Natural Gas...

Claims

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Application Information

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IPC IPC(8): C07C203/00C07C201/04
Inventor 李扬王科谢光全胡玉容范鑫袁小金许红云
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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