A kind of preparation method of H acid monosodium salt

A monosodium salt and sodium salt technology, applied in the preparation of sulfonate, organic chemistry, etc., can solve the problems of high acidity of sulfonation reaction, harsh reaction conditions, high reaction temperature, etc., and achieve the reduction of sulfonation temperature and sulfonation reaction conditions Mild, highly catalytic effect

Active Publication Date: 2015-11-04
JIANGSU MINGSHENG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the cost of the sulfonation reaction is low and the reaction time is short, a large amount of sulfur trioxide needs to be added in the reaction process, and the reaction temperature is high and the reaction conditions are harsh, which easily leads to an increase in side reactions; and the acidity of the sulfonation reaction is relatively high , the high temperature accelerates the corrosion of the equipment

Method used

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  • A kind of preparation method of H acid monosodium salt
  • A kind of preparation method of H acid monosodium salt
  • A kind of preparation method of H acid monosodium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0052] In the flask, drop into refined naphthalene 400g, molybdenum vanadium phosphoheteropolyacid H 4 PMo 11 VO 4015g, then raise the temperature to 80-100°C to melt all the refined naphthalene, then add 350g of sulfuric acid, after the addition, raise the temperature to 110-125°C and keep it warm for 1h, then lower the temperature to below 80°C, add 50g of sulfuric acid, and then cool down to 50 ~60°C, add 500g of sulfur trioxide, control the feeding temperature below 100°C, raise the temperature to 135-145°C for 5 hours after the addition, and keep the temperature for 5 hours. After the reaction, the sulfonated material is obtained, and the acid value is about 60%. - The total yield of trisulfonic acid is 94%, and the content of 1,3,6-naphthalenetrisulfonic acid is 83%.

[0053] After passing the test, control the feed rate of sulfonated material and nitric acid, and continuously enter the nitration reactor at a molar ratio of 1:1.2. Control the temperature of the reactor...

Embodiment 2

[0060] In the flask, drop into refined naphthalene 400g, molybdenum vanadium phosphoheteropolyacid H 4 PMo 11 VO 40 5g, then raise the temperature to 80-100°C to melt all the refined naphthalene, then add 350g of sulfuric acid, after the addition, raise the temperature to 110-125°C and keep it warm for 1h, then lower the temperature to below 80°C, add 50g of sulfuric acid, and then cool down to 50 ~60°C, add 500g of sulfur trioxide, control the feeding temperature below 100°C, raise the temperature to 135-145°C for 5 hours after the addition, and keep the temperature for 5 hours. After the reaction, the sulfonated material is obtained, and the acid value is about 60%. - The total yield of trisulfonic acid is 90%, and the content of 1,3,6-naphthalenetrisulfonic acid is 81%.

[0061] After passing the test, control the feed rate of sulfonated material and nitric acid, and continuously enter the nitration reactor at a molar ratio of 1:1.2. Control the temperature of the reactor...

Embodiment 3

[0066] In the flask, drop into refined naphthalene 400g, molybdenum vanadium phosphoheteropolyacid H 5 PMo 10 VO 40 15g, then raise the temperature to 80-100°C to melt all the refined naphthalene, then add 350g of sulfuric acid, after the addition, raise the temperature to 110-125°C and keep it warm for 1h, then lower the temperature to below 80°C, add 50g of sulfuric acid, and then cool down to 50 ~60°C, add 500g of sulfur trioxide, control the feeding temperature below 100°C, raise the temperature to 135-145°C for 5 hours after the addition, and keep the temperature for 5 hours. After the reaction, the sulfonated material is obtained, and the acid value is about 60%. - The total yield of trisulfonic acid was 92%, and the content of 1,3,6-naphthalenetrisulfonic acid was 81%.

[0067] After passing the test, control the feed rate of sulfonated material and nitric acid, and continuously enter the nitration reactor at a molar ratio of 1:1.2. Control the temperature of the reac...

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Abstract

The invention discloses a preparation method for an H acid monosodium salt. The preparation method comprises the following steps: (1) enabling refined naphthalene and sulfuric acid to be subjected to a sulfonation reaction in the presence of heteropolyacid with a catalyzing amount to obtain a sulfonated product; then adding sulfur trioxide to carry out a secondary sulfonation reaction; reacting completely to obtain a sulfonated material; (2) carrying out a nitration reaction on the sulfonated material and nitric acid to obtain a nitrated material; (3) enabling the nitrated material to be subjected to a hydrogenation reduction reaction in the presence of a hydrogenation catalyst to obtain an amino T acid; (4) adding methanol and sodium hydroxide into the amino T acid and heating and reacting to obtain an alkali melt; and (5) adjusting the pH (Potential of Hydrogen) value of the alkali melt to 3-6 and carrying out acidification and separation to obtain the H acid monosodium salt. According to the preparation method, a specific catalyst is added in a sulfonation step so that the reaction temperature is reduced, a reaction condition is moderate and the corrosion to equipment is reduced.

Description

technical field [0001] The invention belongs to the field of preparation of dye intermediates, in particular to a preparation method of H acid monosodium salt. Background technique [0002] H acid monosodium salt, the Chinese name is 1-amino-8-naphthol-3,6-disulfonic acid monosodium salt, generally with a crystal water, the structure is shown in formula (I), it is an important dye intermediate. H acid monosodium salt is mainly used in the production of acid dyes, direct dyes or reactive dyes, such as acid magenta 6B, acid scarlet G, acid black 10B, direct black, reactive brilliant red K-2BP, reactive violet K-3R , Reactive dark blue K-R and other more than 90 kinds of dyes, these dyes are used in wool spinning and cotton fabrics with good dyeing effect; in addition, monosodium salt of H acid can also be used in the production of medicines. [0003] [0004] At present, the monosodium salt of H acid is mainly produced through the following steps: (1) sulfonation of napht...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/50C07C303/32
Inventor 阮福坤阮国胜郭理想叶华明
Owner JIANGSU MINGSHENG CHEM
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