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Method and device capable of continuously preparing nitrous acid ester

A technology of nitrite and nitrite, which is applied in the chemical industry, can solve the problems of tail gas pollution safety hazards, waste water, large inorganic salts, etc., and achieve the effects of continuous process, low energy consumption and convenient operation

Active Publication Date: 2016-01-13
SHANDONG LANGHENG CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the deficiencies of the prior art, the present application provides a method and device for continuously preparing nitrite, which solves the problems of a large amount of inorganic salt waste water, tail gas pollution and major safety hazards in the prior art during the preparation of nitrite

Method used

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  • Method and device capable of continuously preparing nitrous acid ester
  • Method and device capable of continuously preparing nitrous acid ester

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Experimental program
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Effect test

Embodiment 1

[0030] This embodiment provides a kind of device for continuously preparing nitrite, as figure 2 Shown, comprise bipolar membrane electrodialyzer 1, the entrance of bipolar membrane electrodialyzer 1 is connected with alcohol solution temporary storage tank 2, water tank 3 and nitrite storage tank 4 respectively, the bipolar membrane electrodialyzer 1 The outlets are respectively connected to the residual nitrite solution collection tank 5, the alkali solution concentration section 6 and the nitrite reaction mixed liquid treatment section 7;

[0031] The residual nitrite solution collection tank 5 is connected to the nitrite solution storage tank 4 through the nitrite solution batching kettle 8;

[0032] The post-treatment section 7 of the reaction mixture containing nitrite is connected to the gas-liquid separator 9 and the liquid-liquid separator 10; the gas-liquid separator 9 is provided with a gas ester collection section 11, and the gas-liquid separator 9 is also mixed w...

Embodiment 2

[0037] This embodiment provides a kind of method for continuously preparing nitrite, and this method adopts the device among the embodiment 1, combines figure 1 and figure 2 , wherein the bipolar membrane electrodialyzer is composed of multiple modules, all the chambers formed by the positive membrane and the negative side of the bipolar membrane are connected in parallel and have an inlet a and an outlet a; all the chambers formed by the negative membrane and the positive side of the bipolar membrane are connected in parallel And there are inlet b and outlet b; all the chambers composed of anion and cation membranes are connected in parallel and have inlet c and outlet c; inlet a, inlet b and inlet c of the bipolar membrane electrodialyzer are temporarily stored with the alcohol solution respectively Tank, water tank and nitrite storage tank are connected, outlet a, outlet b and outlet c of the bipolar membrane electrodialyzer are respectively connected with the post-treatme...

Embodiment 3

[0044] Present embodiment provides a kind of method for continuously preparing ethyl nitrite, as figure 1 As shown, the method specifically includes the following steps:

[0045] Step 1, the 30% ethanol aqueous solution is cooled to -5°C through the heat exchanger and pumped into the bipolar membrane electrodialyzer from the inlet a of the bipolar membrane electrodialyzer, and the water is cooled to 1-4°C from the bipolar membrane electrodialyzer The inlet b of the dialyzer is pumped into the bipolar membrane electrodialyzer, and the 15% sodium nitrite solution is cooled to -5°C through the heat exchanger and pumped into the bipolar membrane electrodialyzer from the inlet c of the bipolar membrane electrodialyzer Device, add a voltage of 1.0V direct current to the bipolar membrane electrodialyzer;

[0046] Step 2: The sodium nitrite solution passes through the intermediate chamber composed of the anion and yang membranes. Under the action of a direct current electric field, t...

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Abstract

The invention provides a method and device capable of continuously preparing nitrous acid ester. The method comprises the following steps: taking a nitrite solution and an alcohol solution as the raw materials, individually introducing the nitrite solution and alcohol solution into a bipolar membrane electrodialysis device to carry out reactions to obtain three products: reaction mixed liquid containing nitrous acid ester, a residual nitrite solution, and an alkali solution; recovering the residual nitrite as raw materials for cycle use; recovering the alkali solution; making the reaction mixed liquid containing nitrous acid ester go through a gas-liquid separator or a liquid-liquid separator to obtain nitrous acid ester and an alcohol solution, collecting the target product namely nitrous acid ester, and recovering the alcohol solution as raw materials for cycle use. The provided method does not generate waste gas and waste liquid, the produced alkali liquid can be recovered for industrial production, the generated mother liquor can be completely recovered and reutilized in the reaction system, the production technology is environment-friendly, the reaction temperature is low, the reaction process is safe, and no safety hazard exists.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to nitrite, in particular to a method and device for continuously preparing nitrite. Background technique [0002] Nitrite is an important raw material for the synthesis of sodium azide, oxalate, ethylene glycol, high-purity nitrite and other products. The commonly used production method is to react sodium nitrite with sulfuric acid to generate nitrous acid, and then regenerate it in the reaction system. Reaction with alcohol to generate nitrite, this method will produce a large amount of by-product sodium sulfate wastewater, which is very difficult to treat with conventional methods, and the energy consumption is high and the pollution is large. The prior art discloses a method for synthesizing nitrite by ammonium oxidation for the manufacture of products such as diethyl oxalate and sodium azide. This method has low energy consumption and no high-salt wastewater, but the investment in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C203/00C07C201/04
Inventor 刘湛刘林学郝光顺张明英李建民
Owner SHANDONG LANGHENG CHEM CO LTD
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