Method for green production of germanium tetrachloride from germanium mud
A germanium tetrachloride and green production technology, applied in the direction of germanium halide, etc., can solve the problems of blocked pipelines and low direct yield, achieve uniform heating speed, improve reaction efficiency, and improve mixing effect
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Embodiment 1
[0024] The invention is a method for green production of germanium tetrachloride from germanium mud, comprising the following steps:
[0025] S1: germanium mud pretreatment, the germanium mud is ground into fine particles through a ball mill, and the particle size of germanium mud grinding is set to 80-100 mesh;
[0026] S2: Slurry germanium and heat, the germanium slurry ground in S1 is mixed with water at a ratio of 1:3, that is, 1kg of germanium slurry is added to 3L of water, and then microwave heating is used to raise the temperature to 65°C and keep it warm 3min, the heating rate is set at 8~10℃ / min;
[0027] S3: Add 35% hydrogen peroxide solution dropwise for oxidation, slowly add 35% hydrogen peroxide solution dropwise to the slurry after heat preservation in S2, germanium mud and 35% hydrogen peroxide solution are added in a ratio of 1:3, that is, 1 kg Add 3L35% hydrogen peroxide solution to the germanium mud, and add sodium hydroxide during the whole reaction proces...
Embodiment 2
[0031] The invention is a method for green production of germanium tetrachloride from germanium mud, comprising the following steps:
[0032] S1: germanium mud pretreatment, the germanium mud is ground into fine particles through a ball mill, and the particle size of germanium mud grinding is set to 80-100 mesh;
[0033] S2: Slurry germanium and heat, the germanium slurry ground in S1 is mixed with water at a ratio of 1:3.5, that is, 1kg of germanium slurry is added to 3.5L of water, and then microwave heating is used to raise the temperature to 62.5°C, and Keep warm for 4 minutes, and set the heating rate at 8-10°C / min;
[0034] S3: Add 35% hydrogen peroxide solution dropwise for oxidation, slowly add 35% hydrogen peroxide solution dropwise to the slurry after heat preservation in S2, germanium mud and 35% hydrogen peroxide solution are added in a ratio of 1:3.5, that is, 1 kg Add 3.5L 35% hydrogen peroxide solution to the germanium mud, and add sodium hydroxide during the w...
Embodiment 3
[0038] The invention is a method for green production of germanium tetrachloride from germanium mud, comprising the following steps:
[0039] S1: germanium mud pretreatment, the germanium mud is ground into fine particles through a ball mill, and the particle size of germanium mud grinding is set to 80-100 mesh;
[0040] S2: Slurry germanium and heat. Add water to slurry the ground germanium slurry in S1 at a ratio of 1:4, that is, add 4L water to 1㎏ germanium slurry, and then use microwave heating to raise the temperature to 60°C and keep it warm. 5min, the heating rate is set at 8-10°C / min;
[0041] S3: Add 35% hydrogen peroxide solution dropwise for oxidation, slowly add 35% hydrogen peroxide solution dropwise to the slurry after heat preservation in S2, germanium mud and 35% hydrogen peroxide solution are added in a ratio of 1:4, that is, 1 kg Add 4L 35% hydrogen peroxide solution to the germanium mud, and add sodium hydroxide during the whole reaction process to keep the...
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