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Method for preparing nitrosonaphthol cobalt reagent

A technology of nitrosonaphthol and cobalt reagents, which is applied in the field of organic compound preparation, can solve problems such as low yield and complicated process, and achieve the effect of increasing reaction yield

Inactive Publication Date: 2010-11-24
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of existing nitrosonaphthols has the problems of complicated process and low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A kind of preparation method of cobalt reagent nitrosonaphthol, its preparation step is:

[0016] (1) Reaction: In a 1000 ml reactor with cooling device, electric stirring, thermometer, water circulation condenser and immersion type dropping funnel, drop into 500 milliliters of water, 15 grams of sodium hydroxide successively, open the cooling device The system is cooled to zero degrees Celsius; then slowly add 100 grams of 2-naphthol and 50 grams of sodium nitrite, fully stir until the material is completely dissolved, then slowly add 50% sulfuric acid dropwise through the immersion type dropping funnel, During this process, the temperature of the system is guaranteed not to exceed 2 degrees Celsius by controlling the speed of adding sulfuric acid. While feeding, use Congo red test paper to detect the pH of the system. Stop adding until the Congo red test paper turns blue, and continue stirring after the addition is complete. 40-60 minutes;

[0017] (2) Washing materi...

Embodiment 2

[0021] (1) Reaction: In a 1000 ml reactor with cooling device, electric stirring, thermometer, water circulation condenser and immersion type dropping funnel, drop into 500 milliliters of water, 17 grams of sodium hydroxide successively, open the cooling device The system is cooled to zero degrees Celsius; then slowly add 100 grams of 2-naphthol and 50 grams of sodium nitrite, fully stir until the material is completely dissolved, then slowly add 50% sulfuric acid dropwise through the immersion type dropping funnel, During this process, the temperature of the system is guaranteed not to exceed 2 degrees Celsius by controlling the speed of adding sulfuric acid. While feeding, use Congo red test paper to detect the pH of the system. Stop adding until the Congo red test paper turns blue, and continue stirring after the addition is complete. 40-60 minutes;

[0022] (2) Washing material: leave the above reaction solution overnight, filter and separate the yellow solid in the reacti...

Embodiment 3

[0026] (1) Reaction: In a 1000 ml reactor with cooling device, electric stirring, thermometer, water circulation condenser and immersion type dropping funnel, drop into 500 milliliters of water, 20 grams of sodium hydroxide successively, open the cooling device Cool the system to zero degrees Celsius, then slowly add 100 grams of 2-naphthol and 50 grams of sodium nitrite, fully stir until the materials are completely dissolved; then slowly add 50% sulfuric acid dropwise through the invasive dropping funnel, During this process, the temperature of the system is guaranteed not to exceed 2 degrees Celsius by controlling the speed of adding sulfuric acid. While feeding, use Congo red test paper to detect the pH of the system. Stop adding until the Congo red test paper turns blue, and continue stirring after the addition is complete. 40-60 minutes;

[0027] (2) Washing material: leave the above reaction solution overnight, filter and separate the yellow solid in the reaction soluti...

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Abstract

The invention relates to a method for preparing a nitrosonaphthol cobalt reagent, which comprises the following steps of: (1) adding water and sodium hydroxide into a reactor in turn, then slowly adding 2-naphthol and sodium nitrite into the container, slowly dropping 50 percent sulfuric acid into the container through an immersion type dropping funnel, stopping dropping the sulfuric acid till a piece of congo red test paper becomes blue, and continuously stirring the mixture for 40 to 40 minutes after the sulfuric acid is completely added; (2) filtering and separating yellow solid in the reaction solution from the system, filtering and separating a product, detecting the pH value of the aqueous phase till neutrality, adding ethanol into filter cakes washed by deionized water with filtering, rinsing the filter cakes at one time and naturally drilling the filter cakes; and (3) adding the naturally-dried crude cobalt reagent product into petroleum ether in an amount which is 10-15 times the weight of the naturally-dried crude cobalt reagent product, filtering crystals, and naturally drying the crystals again to obtain the nitrosonaphthol cobalt reagent. The method determines the optimal concentrations of various reactants containing the 2-naphthol, the sodium nitrite and the sodium hydroxide by comparative study on the synthesizing process of the nitrosonaphthol cobalt reagent, so the method improves the reaction yield and is more suitable for the requirement of industrial production.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a preparation method of cobalt reagent nitrosonaphthol Background technique [0002] Cobalt reagent nitrosonaphthol is one of the mass-produced products at home and abroad. It is widely used as a color reagent for the photometric determination of cobalt, palladium, and zirconium, and as a co-factor for enriching chromium ions, cobalt ions, and ferrous ions. Precipitating agent is also used as an extraction agent for silver, lead, cobalt, copper, nickel and other ions, or a precipitant for the determination of cobalt by weighing method, and is also used as an intermediate in organic synthesis. However, the existing preparation of nitrosonaphthol has the problems of complex process and low yield. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies in the prior art and provide a method for preparing cobalt reagent nit...

Claims

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Application Information

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IPC IPC(8): C07C207/04C07C201/00
Inventor 徐博刚
Owner TIANJIN CHEM REAGENT RES INST
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