A method for separating p-chlorobromobenzene and o-chlorobromobenzene by suspension melting crystallization
A suspension melting crystallization, chlorobromobenzene technology, applied in chemical instruments and methods, organic chemistry, halogenated hydrocarbon preparation and other directions, can solve problems such as poor separation effect, and achieve the effects of cost saving, less environmental pollution, and reduced energy consumption
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Embodiment 1
[0026] A method for separating p-chlorobromobenzene and o-chlorobromobenzene by suspension melting crystallization method:
[0027] Step 1. Ultrasonic disperse the solid-liquid mixture of o-chlorobromobenzene and p-chlorobromobenzene with a p-chlorobromobenzene content of 50% for 30 minutes to obtain a dispersion; add the dispersion to a melting crystallizer, heat to 60°C, get mixed melt;
[0028] Step 2, cooling the mixed molten liquid to 55°C and maintaining it for 30 minutes, then cooling to -2°C at a cooling rate of 0.2°C / min, and growing crystals for 2 hours to obtain crude crystals of p-chlorobromobenzene;
[0029] Step 3. The crude p-chlorobromobenzene crystals are heated up to 4°C at a heating rate of 0.3°C / min, sweated, and maintained for 1.5h to obtain pure p-chlorobromobenzene crystals, which are then suction filtered, washed with water, and dried to obtain p-chlorobromobenzene For bromobenzene products, the discharged crystallization mother liquor is collected and...
Embodiment 2
[0031] A method for separating p-chlorobromobenzene and o-chlorobromobenzene by suspension melting crystallization method:
[0032] Step 1. Ultrasonic disperse the solid-liquid mixture of o-chlorobromobenzene and p-chlorobromobenzene with a p-chlorobromobenzene content of 50% for 30 minutes to obtain a dispersion; add the dispersion to a melting crystallizer, heat to 60°C, get mixed melt;
[0033] Step 2: Cool down the mixed molten liquid to 55°C, maintain it for 30min, then cool down to -2°C at a cooling rate of 0.2°C / min, grow the crystal for 2h, suction filter, wash with water, and dry to obtain p-chlorobromobenzene product, The discharged crystallization mother liquor is collected and mixed for recycling. The yield of p-chlorobromobenzene is 66.1%, and the purity is 99.54%.
Embodiment 3
[0035] A method for separating p-chlorobromobenzene and o-chlorobromobenzene by suspension melting crystallization method:
[0036] Step 1. Ultrasonic disperse the solid-liquid mixture of o-chlorobromobenzene and p-chlorobromobenzene with a p-chlorobromobenzene content of 50% for 35 minutes to obtain a dispersion; add the dispersion to a melting crystallizer, heat to 75°C, get mixed melt;
[0037] Step 2. Cool the mixed molten liquid to -10°C at a cooling rate of 0.5°C / min, grow crystals for 6 hours, suction filter, wash with water, and dry to obtain p-chlorobromobenzene products, collect and mix the discharged crystallization mother liquor, and circulate use. The yield of p-chlorobromobenzene is 55.4%, and the purity is 99.04%.
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