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New production method for azodicarbonamide

A technology of azodicarbonamide and manufacturing method, which is applied in electrolysis process, organic chemistry, electrolysis components, etc., can solve the problems of economical benefit and waste of price electricity, etc.

Active Publication Date: 2017-05-31
HANGZHOU HI TECH FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of this patent document has a huge problem that a large amount of expensive electricity is wasted in manufacturing, and it cannot be said to be an economically advantageous method or a method that responds to the needs of the times.

Method used

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  • New production method for azodicarbonamide
  • New production method for azodicarbonamide
  • New production method for azodicarbonamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0084] Hereinafter, the present invention will be described in more detail using examples, but the present invention is not limited to these examples.

[0085] The azodicarbonamide obtained in each of the following examples passes through infrared absorption spectrum (IR) and proton nuclear magnetic resonance spectrum ( 1 H-NMR) for identification.

[0086] IR(KBr): 3337, 3187cm -1 (N-H telescopic), 1743, 1731cm -1 (C=O expansion and contraction), 1637cm -1 (N-H variable angle), 1369, 1331cm -1 (C-N telescopic).

[0087] 1 H-NMR(D6-DMSO): δ8.02(s, 2H, NH), 7.97(s, 2H, NH).

[0088] Quantification of unreacted urea in each of the following examples was performed by high performance liquid chromatography.

[0089] The analysis conditions of the high performance liquid chromatography are as follows.

[0090] column:

[0091] Mobile phase: 10mM acetic acid in water

[0092] Flow rate: 1ml / min

[0093] Detection wavelength: 205nm

[0094] The conversion rate in the fo...

reference example 1

[0099] In a reaction vessel equipped with a stirrer and a thermometer, 75 g (1.25 mol) of urea was dissolved in 150 ml of water, and 321 ml (1.25 mol) of 29% sodium hypochlorite aqueous solution was added dropwise at 10° C. with stirring over 1 hour. Take a sample, add potassium iodide and acetic acid (1:1), and quickly carry out 0.1N-sodium thiosulfate titration. As a result of titration analysis, it was confirmed that the yield of monochlorourea was 98.4%. When ultraviolet analysis was performed, absorption at 244 nm peculiar to monochlorourea was confirmed.

reference example 2

[0101] Based on the addition of 10.7% NaOCl aqueous solution (as Cl 2 The preparation of bromourea solution (NaOCl: HCl: urea: the molar ratio of NaBr 1: 2.2: 37.7: 0.8) of 38% aqueous solution (weight %) of NaBr

[0102] In a 250ml round bottom flask equipped with a stirring bar, dropping funnel and thermometer, 46.04g of urea (767mmol) was dissolved in 30.6g of H 2 O, followed by the addition of 5.4 g of 32% HCl (47.2 mmol) (with heat generation upon cooling). A solution of urea hydrochloride was obtained. 13.5 g of 10.7% NaOCl aqueous solution (with Cl 2 % by weight, 20.3 mmol) was added to the addition funnel, and 4.84 g of 38% NaBr solution was added to another addition funnel. The NaOCl solution was added to the urea hydrochloride solution and 38% NaBr aqueous solution was added to this solution 1 min later. When ultraviolet analysis is carried out, bromureon-specific absorption at 275 nm is shown. Take a sample, add potassium iodide and acetic acid (1:1), and quick...

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Abstract

Provided is an economical, safe, and more environmentally-friendly production method for azodicarbonamide. According to the present invention, in a homogeneous system or heterogeneous miscible system of water or an organic solvent or an ionic solution, and an organic solvent and / or an ionic solution and water, azodicarbonamide is produced by using hydrogen peroxide in urea and reacting active chlorine or active chlorine ions and an active bromine compound such as active bromine or active bromine ions and / or an active form derived from hydrogen peroxide, or by electrolytically oxidizing an intermediate as desired to obtain a target, and recycling and using post-reaction byproducts.

Description

technical field [0001] The invention relates to a production method for obtaining azodicarbonamide by using urea active derivatives and structures. Background technique [0002] Azodicarbonamide is a useful compound widely used as a blowing agent from the viewpoint of its excellent decomposition behavior, physical properties, and chemical properties. [0003] The most commonly implemented conventional production method is: as shown in the following reaction formula (1), azodimethazine is produced by a several-stage reaction including the reaction of hydrazine hydrate produced from urea or ammonia as a raw material and 2 moles of urea Amide method (Patent Document 1). This conventional production method causes wasteful consumption of raw materials that do not contribute to the molecular structure of the target substance, azodicarbonamide, and causes an increase in cost. In addition, generation of a large amount of ammonia by-produced, carbon dioxide gas causing global warmi...

Claims

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Application Information

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IPC IPC(8): C07C281/20C25B3/23
CPCC07C281/20
Inventor 谷口正俊
Owner HANGZHOU HI TECH FINE CHEM
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