Method for directly producing water soluble aniline black
A water-soluble nigrosine, direct technology, applied in the direction of benzene azine dyes, organic chemistry, etc., can solve the problems of long production process cycle, large heat energy waste, high energy consumption, etc., to improve labor production efficiency, reduce waste water discharge, Energy and labor saving effects
Inactive Publication Date: 2012-09-26
严纪一
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Problems solved by technology
The production process has a long cycle and high energy consumption. It takes 2.5 tons of standard coal to produce one ton of water-soluble nigrosine, which results in a large waste of heat energy.
Method used
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[0029] The present invention discloses a method for directly producing water-soluble nigrosine, and its specific steps are:
[0030] Step 1. Condensate aniline and nitrobenzene under the catalysis of ferric chloride;
[0031] Step 2: Naturally cool the condensed mixture to room temperature;
[0032] Step 3: pulverize the naturally cooled mixture and directly throw it into sulfuric acid for sulfonation reaction;
[0033] Step 4. Put the sulfonated mixture in cold water for isolation;
[0034] Step 5, the separated mixture is subjected to solid-liquid separation and water washing, and then dehydrated;
[0035] Step 6, the dehydrated mixture is neutralized with sodium hydroxide or sodium carbonate;
[0036] In step 7, the neutralized mixture is dried to obtain particulate water-soluble aniline black.
[0037] On the basis of the above technical solution, it also includes the following steps:
[0038] Step 8, pulverize the particulate water-soluble aniline black to obtain a powdered water-solub...
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The invention discloses a method for directly producing water soluble aniline black, and relates to the preparation of an azine acid dye. The method particularly comprises the following steps of: 1, performing condensation reaction on aniline and nitrobenzene in the presence of iron trichloride serving as a catalyst; 2, naturally cooling the condensed mixture to normal temperature; 3, crushing the naturally cooled mixture and directly putting the crushed mixture into sulfuric acid for sulfonation reaction; 4, placing the sulfonated mixture in cold water for separation; 5, performing solid-liquid separation and washing on the separated mixture and then performing dehydration; 6, neutralizing the dehydrated mixture with sodium hydroxide or sodium carbonate; and 7, drying the neutralized mixture so as to obtain the granular water soluble aniline black. The method for directly producing the water soluble aniline black of the invention simplifies the processing steps, shortens the process period, saves a large amount of energy sources and labor resources, reduces the waste water discharge and greatly improves the labor efficiency and production efficiency.
Description
Technical field [0001] The invention relates to the preparation of azine acid dyes, in particular to a method for directly producing water-soluble nigrosine. Background technique [0002] The molecular formula of the water-soluble nigrosine (index number: [CI]ACID BLACK 2(52420)) in azine acid dyes is C 36 H 26 O 6 N 5 S 2 N a (See figure 1 ), the alias names of water-soluble nigrosine black are: acid particle element, acid particle element NBL, acid skin element NL, acid particle element green, acid black 2; English names are: Acid nigrosine, CIacid black 2, calco nigrosine o 2p , Ci 50420, ci acid black 2, lurazol deep blue eb, nigrosin, nigrosine b, nigrosine wl water soluble, nigrosine wsb; usually in particle or powder form; widely used in wool dyeing (in a strong acid bath, pH control Below 3.5, add Yuan Mingfen as a retarding agent to improve levelness), high-grade ink, silk dyeing (in scouring liquid, adding acetic acid or sulfuric acid to get gray black), leather bottom ...
Claims
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IPC IPC(8): C07D241/46C09B17/02
Inventor 严纪一
Owner 严纪一