Preparation method of 2, 6-dihydroxytoluene in laboratory
A dihydroxytoluene, laboratory technology, applied in 2 fields, can solve the problems of product impurity, high production cost, great human injury, etc., and achieve the effect of stable product quality, low production cost and simple operation
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Embodiment 1
[0047] Add 667g of 30% fuming sulfuric acid to the reaction flask, add 136g of p-toluic acid under stirring, raise the temperature to 180°C-195°C, keep the temperature for 5 hours, cool the reaction solution to below 100°C, add it to ice water, and cool Add sodium sulfate 1.8 times the mass of the raw material at 42°C-50°C; keep stirring at 42°C-50°C for 4 hours, cool to 25°C-30°C and centrifuge to obtain 388g of wet product;
[0048] Add 65g of water, 130g of sodium hydroxide and 130g of potassium hydroxide to an alkali fusion kettle, heat to 230°C and start stirring, slowly add 388g of sulfonated product when the temperature rises to 270°C; keep warm for 2.5 hours at 270°C-275°C Afterwards, hydrolyze with 600g of water, cool to 50°C and acidify with sulfuric acid until the pH value is 6-7, and filter the alkali fusion product when the temperature is lowered to 35°C, refine the alkali fusion product with water to adjust the crystallinity to 50°C, decolorize and filter the filt...
Embodiment 2
[0051] Add 667g of 30% fuming sulfuric acid to the reaction bottle, add 136g of p-toluic acid under stirring, raise the temperature to 185°C-198°C, keep it warm for 5 hours, cool the reaction solution to below 100°C, add it to ice water, and cool Add 245g of sodium sulfate to 42°C-50°C; keep stirring at 42°C-50°C for 4 hours, cool to 25°C-30°C and centrifuge. A small amount of sodium sulfate aqueous solution was rinsed to obtain 390 g of wet product;
[0052]Add 60g of water, 130g of sodium hydroxide and 130g of potassium hydroxide to the alkali fusion kettle, heat to 230°C and start stirring, add 390g of sulfonated product when the temperature rises to 270°C, keep it at 270°C-275°C for 2.5 hours before use Hydrolyze 600g of water, cool to 50°C with water, then acidify with sulfuric acid to pH 6-7, and filter to obtain alkali fusion product when the temperature is lowered to 35°C, adjust the crystallinity of the refined alkali fusion product to 50°C, decolorize and filter the ...
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