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6.
Production process
In the mixing tank, 180kg of concentrated nitric acid and 380kg of concentrated sulfuric acid are mixed to form a mixed acid for later use
.
Add 300kg of ethylbenzene into the enamel reactor, and when the temperature is raised to 32°C±2°C, start to slowly add the prepared mixed acid dropwise
The oxidation reaction is carried out in an autoclave that can withstand 1.
0MPa
.
First, 600 kg of p-nitroethylbenzene prepared above was put into a 1000 L autoclave, and then 50 g of cobalt stearate and 60 g of manganese acetate were added as catalysts
Stop air flow and relieve pressure
.
When cooled to 80°C, the reaction materials were transferred to the neutralization kettle, and sodium carbonate was added to neutralize the pH to 7-8
7.
Laboratory preparation method
Put 200mL of water, 50g of magnesium nitrate hexahydrate and 15.
1g of p-nitroethylbenzene in a three-necked flask, stir and heat to 60°C
.
Add 25g of finely ground potassium permanganate in four times, and add the next batch when the purple color of the solution disappears
8.
Product Standard
9.
Quality inspection
Assay: accurately weigh 1.
2g of the sample, dissolve it with ethanol, and dilute to 100mL
.
Weigh another 1.
Take 100mL of 2,4-dinitrophenylhydrazine solution in a 600mL beaker, and then take 100mL of sample solution and add
.
After stirring for 5-10 minutes, add 400 mL of water, keep it in an oven at 80°C for 3 minutes, filter in a constant-volume pore funnel, and wash with 20 mL of 1mo/L sulfuric acid
In the formula: W 1 —— sample mass, g;
W 2 ——product quality, g
.
Gas chromatography can also be used to determine the content
.
10.
Product use
It is used as an intermediate for organic synthesis and pharmaceutical synthesis (such as synmycin and chloramphenicol); it is also used for the synthesis of pesticides, dyes and perfumes
.
11.
Safety measures
(1) This product is toxic, and mixed acid is used in production
.
The equipment must be closed, and the workshop must be well ventilated
(2) Packed in iron drum lined with plastic bag, stored in a cool, dry, ventilated place, protected from heat, moisture, and sunlight, and sealed
.
Related links: Production principle and technical formula of p-nitroacetophenone