Method for producing high-purity phosphoric acid crystal
A production method, phosphoric acid technology, applied in phosphoric acid, phosphorus oxyacids, chemical instruments and methods, etc., to achieve low production costs, inhibit secondary nucleation, and reduce production costs
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Embodiment 1
[0021] (1) Preparation of seed crystals:
[0022] Take 500gH 3 PO 4 Add electronic grade phosphoric acid with a mass percentage of 99% into a 1000mL three-port boron glass crystallizer, connect a stirrer, a drying tube, and a cooling system, and quickly cool down to ≤20-35°C under stirring, and obtain crystal seeds for explosive crystallization;
[0023] (2) Crystallization:
[0024] Take 600g H 3 PO 4 Add thermal phosphoric acid with a mass percentage of 99% into a 1000mL boron glass crystallizer, connect the stirrer, drying pipe, and cooling system, start stirring, the stirring rate is 400rpm, and when the temperature of the material is controlled at 42°C, add 60g of crystal seeds. Keep warm for 2 hours, then program cooling, the cooling rate is 5°C / h, cool down for 1h, and then press the cooling rate of 2°C / h, cool down for 1h, cool to 35°C, keep the crystal for 2h, then centrifugally filter, and the obtained crystals are washed with an appropriate amount of high-purity...
Embodiment 2
[0032] (1) Preparation of seed crystals:
[0033] With embodiment 1;
[0034] (2) Crystallization:
[0035] Take 600g H 3 PO 4 Add thermal food-grade phosphoric acid with a mass percentage of 96.5% into a 1000mL boron glass crystallizer, connect the stirrer, drying pipe, and cooling system, start stirring at a stirring rate of 300rpm, and add 6g of seed crystals when the temperature of the material is controlled at 28°C , keep warm for 0.5h, then program cooling, the cooling rate is 2°C / h, cool down for 0.5h, then cool down at a cooling rate of 1°C / h, cool down for 1h, cool to 26°C, keep the crystal for 1.5h, and centrifuge to obtain the crystal Wash with an appropriate amount of high-purity phosphoric acid solution to obtain 300 g of orthophosphoric acid crystals, with a phosphoric acid yield of 49.5%.
[0036] table 3
[0037]
[0038] (3) Recrystallization:
[0039] Take 300g of the above-mentioned orthophosphoric acid crystals and add them to a 500mL boron glass c...
Embodiment 3
[0044] (1) Preparation of seed crystals:
[0045] With embodiment 1;
[0046] (2) Crystallization:
[0047] Take 600g H 3 PO 4 Add 98% wet-purified phosphoric acid into a 1000mL boron glass crystallizer, connect the stirrer, drying pipe, and cooling system, start stirring at a stirring rate of 400rpm, and control the temperature of the material at 39°C. Add 30g of crystals and keep The temperature is 0.1h, then program cooling, the cooling rate is 2°C / h, the temperature is lowered for 2h, and then the cooling rate is 2°C / h, the temperature is lowered for 1.5h, cooled to 32°C, and the crystal is incubated for 0.5h, and centrifugal filtration is obtained. An appropriate amount of high-purity water was washed to obtain 410 g of orthophosphoric acid crystals, and the yield of phosphoric acid was 65.08%.
[0048] (3) Recrystallization:
[0049] Take 300g of the above-mentioned orthophosphoric acid crystals and add them to a 500mL boron glass crystallizer, add 5g of ultrapure w...
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Abstract
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