Organic-matter nitrosoation method with no production of nitric oxide waste gas

A technology of organic matter and nitrogen oxide, which is applied in the field of clean chemical technology, can solve the problems of wasting raw materials, serious air pollution, and poor treatment effect, and achieve the effects of eliminating nitrogen oxide waste gas, saving nitrite raw materials, and eliminating pollution.

Inactive Publication Date: 2010-05-26
陈学玺
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] NO 2 NO and NO are both volatile gases, which are easily volatilized from the reaction system, which not only increases the consumption of raw materials for the nitrosation reaction, but also causes great damage to the atmosphere due to the volatilized nitrogen oxide gas
[0008] (3) In order to reduce the environmental pollution caused by nitrosation side reac

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: The clean nitrosation method of 4-nitro-m-cresol

[0019] Mix 240ml of water and 66ml of 65% concentrated nitric acid to make 18% nitric acid solution, add it into a four-necked flask equipped with a stirrer, a thermometer, and a drop-dropping device, cool the solution to (0-3)°C with an ice-water bath, add 0.5 g of phase transfer catalyst triethylbenzyl ammonium chloride (TEBA). Prepare a sodium nitrite solution with 20g of sodium nitrite and 40ml of water, and add the solution to the dripping device. Add 27.5g m-cresol in another dripping device under the liquid, add sodium nitrite solution 10ml (about 1 / 6 of the total amount) to the reaction solution earlier, after stirring for 5min, open the dripping device under the liquid, Under the reaction solution, m-cresol and sodium nitrite solution were added dropwise at the same time. Control a certain rate of addition so that the temperature of the reaction solution does not exceed 5°C. Finally, the sodium ...

Embodiment 2

[0021] Example 2: Clean nitrosation method of 1,3-dimethyl 4-imino-5-isonitrosourazine.

[0022] Inhale dimethylcyanoacetylurea into the ring-sealing tank, start stirring and slowly add liquid caustic soda, adjust the pH to 9.1~11.5, when 1,3-dimethyl-4-imidocarbazine is precipitated, heat up to 90-100°C , keep the pH at 9.1-11.5, react at 90-98°C for 10-15 minutes, and measure the end-point pH at 9.1-11.5 after the reaction. Lower the temperature to 20-60°C, and then add the pre-dissolved sodium nitrite aqueous solution.

[0023] Add dilute sulfuric acid (50-60%) into the sub-chemical tank first, turn on the cooling water and stir, slowly press in the mixture of 1,3-dimethyl-4-imidecarbazine and sodium nitrite, and control the pH to 3.1 ~3.5, temperature ≤65°C, react for 10-15 minutes, check with starch-potassium iodide test solution, the end point should be blue. If the end point is not reached, sodium nitrite should be added to generate 1,3-dimethyl 4-imino-5-isonitrosour...

Embodiment 3

[0024] Example 3: Clean nitrosation method of 2,5-dinitroso-2,5,7,9-tetraazabicyclonon-8-one.

[0025] Weigh 2,5,7,9-tetraazabicyclonon-8-one hydrochloride with a melting point of 182-184°C and dissolve it in water, add concentrated hydrochloric acid dropwise under stirring, and cool with an ice-water bath to lower the solution temperature to 0-10°C. Close the reactor, slowly add dropwise a solution made of 20g sodium nitrite and 30ml water, keep it warm at 0-10°C for reaction after the addition, filter, wash twice with 30ml water, ethanol, ether, and vacuum dry to obtain 2.7 g of the product 2,5-dinitroso-2,5,7,9-tetraazabicyclononan-8-one.

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PUM

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Abstract

The invention provides an organic-matter nitrosoation method with no production of nitric oxide waste gas, which belongs to the technical field of clean chemical processes and comprises nitrosoation reaction. The method is characterized in that the nitrosoation reaction is performed in closed space, and the highest pressure in the closed space is 0.4 to 0.6 MPa. The method prevents nitrous acid from being decomposed by sealing and pressurizing equipment so as to avoid producing nitric oxide waste gas. The method has the advantages of ensuring no emission of nitric oxide gas during production, producing no environmental pollution, saving raw material and reducing production cost.

Description

technical field [0001] The invention belongs to the technical field of clean chemical technology, and in particular relates to a new method for nitrosation of organic matter without generating nitrogen oxide waste gas. Background technique [0002] Carrying out nitrosation reaction on benzene ring, cycloalkane ring or pyridine ring, connecting some parts of these compounds with nitroso groups, can make these compounds produce specific functions or continue to react to form compounds with nitrogen atoms. [0003] At present, many nitrosation reactions are carried out as follows: [0004] (1) Mix nitrite (such as sodium nitrite) with the nitrated substance, stir well with the reaction medium (solvent or water), and then drop inorganic acid (sulfuric acid, hydrochloric acid or nitric acid) into it to produce a chemical reaction. The result of the chemical reaction is that the nitrous acid produced by nitrite and inorganic acid combines with the ring-shaped organic matter to fo...

Claims

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Application Information

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IPC IPC(8): C07B43/02C07C207/04C07C201/00C07D239/545C07D487/02C07C211/52C07C209/68
Inventor 陈学玺尹进华陈春光
Owner 陈学玺
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