Preparation method of high-purity zinc phosphide
A zinc phosphide and high-purity technology, applied in the direction of phosphide, can solve the problems that zinc and phosphorus cannot be completely combined, the structure of the sealed furnace is complicated, and the product purity is low, so as to achieve low production cost, easy control of reaction conditions, and production The effect of simple equipment
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[0030] The preparation method of high-purity zinc phosphide provided by the invention comprises the following steps:
[0031] Step S1: primary heating synthesis: Weigh zinc powder and red phosphorus powder according to the mass ratio of 3.02~3.16:1 and mix evenly to form a mixture 3, put it into the primary horizontal reaction boat 4, then put the primary horizontal reaction boat 4 into the The first-time quartz tube 1 of flowing inert gas A is connected with the first-time quartz cap 6, and synthesized according to the first-time heating temperature to obtain the first-time synthesized coarse zinc phosphide;
[0032] Step S2: secondary heating to volatilize and remove impurities: crush the coarse zinc phosphide into powder 13, put it into the secondary horizontal reaction boat 14, and then put the secondary horizontal reaction boat 14 into the secondary quartz tube through which the inert gas A flows 11, connect the primary quartz cap 16, remove impurities by volatilization a...
Embodiment 1
[0040] 1) One-time heating synthesis: Weigh 760g of metal zinc powder with a purity of 4N and a particle size of 100 mesh and 241g of red phosphorus powder with a purity of 4N and a particle size of 200 mesh, mix them evenly and put them into the primary horizontal quartz reaction boat 4, and then put the primary horizontal quartz Put the reaction boat 4 into the primary quartz tube 1 with flowing inert gas A, connect the primary quartz cap 6, seal it completely, turn on the heating furnace 2, heat up to 430°C at a heating rate of 40°C / h, keep the temperature for 2 hours, and then close Heating furnace 2, cooling down to room temperature naturally to obtain primary synthetic crude zinc phosphide, the flow rate of inert gas A in the heating and constant temperature stage is 0.06m 3 / h, the flow rate of inert gas A in the cooling stage is 0.02m 3 / h.
[0041] 2) Secondary heating for volatilization and impurity removal: crush the primary synthesized zinc phosphide in a glove bo...
Embodiment 2
[0045] 1) Primary heating synthesis: Weigh 380g of metal zinc powder with a purity of 5N and a particle size of 30 mesh and 123g of red phosphorus powder with a purity of 5N and a particle size of 100 mesh, mix them evenly and put them into the primary horizontal graphite reaction boat 4, and then put the primary horizontal graphite Put the reaction boat 4 into the primary quartz tube 1 with flowing inert gas A, connect the primary quartz cap 6, seal it completely, turn on the heating furnace 2, raise the temperature to 500°C at a rate of 60°C / h, keep the temperature constant for 4 hours, and then close Heating furnace 2, naturally cooled down to room temperature, the flow rate of inert gas A in the heating and constant temperature stage is 0.05m 3 / h, the flow rate of inert gas A in the cooling stage is 0.03m 3 / h, to obtain a synthetic crude zinc phosphide.
[0046] 2) Secondary heating to volatilize and remove impurities: crush the primary synthesized zinc phosphide into a...
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