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6.
Production process
First press 1700L of o-nitroethylbenzene solvent into the sulfonation kettle, and with stirring, pour 400kg 2-naphthol into the sulfonation kettle, and cool to 0°C
.
Inhale chlorosulfonic acid in a vacuum, and stop adding chlorosulfonic acid when the temperature rises to 4°C
Add 1900L of water (including the condensed water vaporized during concentration) into the neutralization pot
.
Under stirring, add 220 kg of sodium carbonate , and add the sulfonate to neutralize
After the liquid separation in the neutralization pot is completed, put the residual liquid of nitroethylbenzene into the rinsing tank, and at the same time add 40kg of liquid caustic soda, and stir for 5-10min
.
Then rinse with warm water until it becomes neutral, and the time is 2.
The concentrated liquid is put into the high-pressure amination reactor, 190kg ammonium sulfite is added , then the stirring is stopped, and the ammonia is passed through under cooling to a total ammonia amount of 210kg, and the temperature is raised to 150°C.
Incubate and amination for 4h
.
While the autoclave is kept warm, 2000L water is placed in an 8000L wooden barrel and heated to 90°C with direct steam
.
After the heat preservation of the autoclave is completed, the vent valve on the autoclave can be opened to pass in the cooled concentrated liquid to recover ammonia, and at the same time let off the interlayer steam of the autoclave
7.
Product Standard
8.
Quality inspection
Content determination: accurately weigh about 20g of the sample (accurately to 0.
001g), add 200mL distilled water and 30mL 10% Na2CO3, stir the glass rod until it is completely dissolved, pour it into a 500mL volumetric flask, add distilled water to dilute to the mark, and shake to prepare Get the sample solution
.
Take 25mL sample solution, inject it into a 600mL beaker, add 100mL 2mol/L sodium acetate solution and 100mL distilled water cooled to 0～5℃, then cool to 0～5℃ in an ice bath, and use 0.
1mol/L under stirring.
L p-nitroaniline diazonium salt standard solution titration
.
The burette is jacketed with an ice tube for cooling
In the formula: c—molar concentration of p-nitroaniline diazonium salt standard solution, mol/L;
V—Volume of p-nitroaniline diazonium salt standard solution consumed by titration, mL;
G——The mass of the sample, g
.
9.
Product use
Mainly used in the dye industry, it is an intermediate of azo dyes, azo pigments and fluorescent whitening agents
.
For the manufacture of J acid, gamma] acid, naphthol AS-SW, Reactive Red K-1613, an organic purple, lithol red, lithol red, optical brighteners leukophor EFG, leukophor EGM and whiteners RBS like
10.
Security measures
(1) The raw material β-naphthol is toxic, has a strong irritating effect on the skin and mucous membranes, is easily absorbed through the skin, and is highly corrosive; chlorosulfonic acid is a first-class inorganic acidic corrosive product, which can cause severe burns in contact with the skin
.
The equipment must be closed, the workshop should be well ventilated, and the operator should wear protective equipment
.
(2) This product is poisonous.
It is packed in a woven bag lined with a plastic bag and stored in a cool, ventilated place to prevent moisture and heat
.
Store and transport as toxic chemicals
.
Related Links: Product performance and production principle of Tobias acid
