CN110256079B - Preparation method of high-purity compact arsenopyrite electrode - Google Patents
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Abstract
The invention discloses a preparation method of a high-purity compact arsenopyrite electrode, which comprises the following steps: selecting arsenopyrite particles; cleaning the selected arsenopyrite particles and drying for later use; grinding the dried arsenopyrite into powder with a particle size of more than 200 meshes, weighing 0.8-1.0g of arsenopyrite powder ore, pressing into arsenopyrite cylinder in a powder tablet press, and wrapping with silver foil; pressing the arsenopyrite cylinder wrapped by the silver foil into boron nitride to prepare a boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil; putting the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil into the pyrophyllite block for high-pressure assembly; heating and pressurizing sintering in a large-cavity press; stripping silver foil on the surface of the sintered sample to prepare a arsenopyrite electrode; the technical problems that experimental research on high-temperature high-pressure electrochemistry of the arsenopyrite requires that arsenopyrite minerals have good pressure maintaining performance, and natural arsenopyrite minerals are difficult to meet conditions are solved.
Description
Technical Field
The invention belongs to the technical field of electrode preparation, and particularly relates to a preparation method of a high-purity compact arsenopyrite electrode.
Background
Arsenopyrite is the most common sulfur and arsenic compound in nature, and weathering of arsenopyrite can cause arsenic release, so that ground surface and underground water are polluted, and the ecological environment and human health are threatened. The research on the electrochemical corrosion behavior of the arsenopyrite in a hydrothermal system is helpful for understanding the generation, composition and change process of the hydrothermal deposit, provides a theoretical basis for high-temperature hydrometallurgy and mineral processing technology, and is closely related to the understanding of geochemical cycle of the elements such as the ductile iron, arsenic and sulfur, mining and natural environment protection.
The arsenopyrite coexists with cassiterite, wolframite and bismuthate in the high-temperature hydrothermal deposit; symbiotic with pyrrhotite, magnetite and chalcopyrite in skarn-type deposits; coexisting with sulfide in the mesophilic hydrothermal deposit. And the electrochemical corrosion process of the arsenopyrite can be interfered by the chemical action of the primary battery among the symbiotic minerals, so that the experimental result is greatly influenced. Therefore, the preparation of pure arsenopyrite electrodes becomes a necessary condition for electrochemical corrosion research. In addition, the experimental research of high-temperature high-pressure electrochemistry carried out on the arsenopyrite requires that arsenopyrite minerals have good pressure maintaining performance, and natural arsenopyrite minerals are difficult to meet the conditions.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the preparation method of the high-purity compact arsenopyrite electrode is provided to solve the technical problems that the preparation of the high-purity arsenopyrite electrode in the prior art becomes a necessary condition for electrochemical corrosion research, experimental research on arsenopyrite by high-temperature high-pressure electrochemistry requires that arsenopyrite minerals have good pressure maintaining performance, natural arsenopyrite minerals are difficult to meet the conditions, and the like.
The technical scheme of the invention is as follows:
a preparation method of a high-purity compact arsenopyrite electrode comprises the following steps:
step 1, selecting arsenopyrite particles;
step 2, cleaning and drying the selected arsenopyrite particles for later use;
step 3, grinding the dried arsenopyrite into powder with the granularity of more than 200 meshes, weighing 0.8-1.0g of arsenopyrite powder ore, pressing the arsenopyrite powder ore into a arsenopyrite cylinder in a powder tablet press, and wrapping the arsenopyrite cylinder by using a silver foil;
step 4, pressing the silver foil wrapped arsenopyrite cylinder into boron nitride to prepare a boron nitride cylinder containing the silver foil wrapped arsenopyrite cylinder;
step 5, putting the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil into a pyrophyllite block for high-pressure assembly;
step 6, heating, pressurizing and sintering in a large-cavity press;
and 7, stripping silver foil on the surface of the sintered sample to prepare the arsenopyrite electrode.
The method for selecting the arsenopyrite particles in the step 1 comprises the following steps: crushing ore containing toxic placer into 40-80 meshes, and selecting the toxic placer with the purity of more than 98% under a binocular microscope.
The method for drying the washed arsenopyrite particles in the step 2 comprises the following steps: ultrasonically cleaning with anhydrous ethanol for 10-20min, taking out, cleaning with anhydrous ethanol, and oven drying at 50 deg.C in a vacuum oven.
The method for preparing the arsenopyrite cylinder in the step 3 comprises the following steps: adding the weighed arsenopyrite powder into a powder tabletting cylindrical die, compacting for 2min in a powder tabletting machine under the condition of 0.5MPa, reversing the die, taking out the arsenopyrite cylinder, and wrapping with a silver foil.
Step 4, the specific method of the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil comprises the following steps: processing boron nitride into a rod shape, cutting a boron nitride cylinder with the same length as the arsenopyrite cylinder, drilling a hole with the same diameter as the arsenopyrite cylinder wrapped by the silver foil on the boron nitride cylinder, pressing the arsenopyrite cylinder wrapped by the silver foil into the hole of the boron nitride cylinder, and covering boron nitride wafers with the thickness of 3-5mm at the upper end and the lower end of the boron nitride cylinder.
Step 5, the method for putting the pyrophyllite block into the high-pressure assembling machine comprises the following steps:
step 5.1, selecting a pyrophyllite square block, and drilling a circular through hole in the center of the pyrophyllite block;
step 5.2, placing a circular stainless steel heating sheet on the inner wall of the through hole;
step 5.3, placing a boron nitride cylinder containing a silver foil wrapped arsenopyrite cylinder in the middle of the stainless steel heating plate, and sealing and compacting the upper end and the lower end by a pyrophyllite plug;
and 5.4, connecting a thermocouple into the pyrophyllite square block.
The method for heating and pressurizing sintering by the large-cavity press in the step 6 comprises the following steps: assembling pyrophyllite blocks under high pressure, placing in a six-axis hinge type cubic press, heating, pressurizing and sintering under the pressure of 0.6-2.0GPa, the temperature of 300-.
The access method of the thermocouple in the high-voltage assembly block comprises the following steps:
preparing a thermocouple: respectively inserting a nickel-chromium wire and a nickel-silicon wire into the double-hole ceramic tube, and welding in a saturated sodium chloride solution with the voltage of 80-200V;
thermocouple access: a hole is drilled in the middle of the side edge of the pyrophyllite square block, a thermocouple is connected into the hole, and the thermocouple is next to the boron nitride cylinder.
The invention has the beneficial effects that:
according to the invention, selected arsenopyrite particles are ground into a powder raw material by using high-temperature ultrahigh-pressure equipment, the interface among crystal particles is eliminated by a melting recrystallization method under the conditions of pressure and temperature of arsenopyrite which exist stably, the crystal particles grow up, the arsenopyrite powder raw material is formed into a compact block material to reach the required hardness and strength, and then the arsenopyrite electrode with high purity and compactness is successfully prepared by mechanical processing and grinding; the technical problem that the electrochemical corrosion result of the arsenopyrite is influenced by the effect of a galvanic cell generated by the symbiosis of a natural arsenopyrite electrode and other sulfide minerals is solved. In addition, the toxic sand mineral electrode has good pressure maintaining performance and can meet the research requirements of high-temperature and high-pressure experiments; the method solves the technical problems that the preparation of a high-purity arsenopyrite electrode in the prior art becomes a necessary condition for electrochemical corrosion research, the experimental research of high-temperature high-pressure electrochemistry on arsenopyrite requires that arsenopyrite minerals have good pressure maintaining performance, and natural arsenopyrite minerals are difficult to meet the conditions.
Detailed Description
Preparation method of high-purity compact arsenopyrite electrode
Step 1, selecting arsenopyrite particles;
step 2, cleaning and drying the selected arsenopyrite particles for later use;
step 3, grinding the dried arsenopyrite into powder with the granularity of more than 200 meshes, weighing 0.8-1.0g of arsenopyrite powder ore, pressing the arsenopyrite powder ore into a arsenopyrite cylinder in a powder tablet press, and wrapping the arsenopyrite cylinder with silver foil;
step 4, pressing the silver foil wrapped arsenopyrite cylinder into boron nitride to prepare a boron nitride cylinder containing the silver foil wrapped arsenopyrite cylinder;
step 5, putting the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil into a pyrophyllite block for high-pressure assembly;
step 6, heating, pressurizing and sintering in a large-cavity press;
and 7, stripping silver foil on the surface of the sintered sample, and preparing the high-purity compact arsenopyrite electrode.
The method for selecting the arsenopyrite particles in the step 1 comprises the following steps: crushing ore containing toxic placer into 40-80 meshes, and selecting the toxic placer with the purity of more than 98% under a binocular microscope.
The method for drying the washed arsenopyrite particles in the step 2 comprises the following steps: ultrasonically cleaning with anhydrous ethanol for 10-20min, taking out, cleaning with anhydrous ethanol, and oven drying in a vacuum oven at 50 deg.C.
The method for preparing the arsenopyrite cylinder in the step 3 comprises the following steps: adding the weighed arsenopyrite powder into a powder tabletting cylindrical die, compacting for 2min in a powder tabletting machine under the condition of 0.5MPa, reversing the die, taking out the arsenopyrite cylinder, and wrapping with a silver foil.
Step 4, the specific method of the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil comprises the following steps: processing boron nitride into a rod with a proper size, cutting out a boron nitride cylinder with the same length as the arsenopyrite cylinder, drilling a hole with the same diameter as the arsenopyrite cylinder wrapped by the silver foil on the boron nitride cylinder, pressing the arsenopyrite cylinder wrapped by the silver foil into the hole of the boron nitride cylinder, and covering boron nitride wafers with the thickness of 3-5mm at the upper end and the lower end of the boron nitride cylinder.
Step 5, the specific operation of putting the pyrophyllite block into the high-pressure assembly is as follows:
step 5.1, selecting a pyrophyllite square block, and drilling a circular through hole in the center of the pyrophyllite block;
step 5.2, placing a circular stainless steel heating sheet on the inner wall of the through hole;
step 5.3, placing a boron nitride cylinder containing a silver foil wrapped arsenopyrite cylinder in the middle of the stainless steel heating plate, and sealing and compacting the upper end and the lower end by a pyrophyllite plug;
and 5.4, connecting a thermocouple into the pyrophyllite square block.
And 6, performing heating and pressurizing sintering on the large-cavity press, namely assembling the pyrophyllite blocks at high pressure, putting the assembled pyrophyllite blocks into a DS-6 x 1400t six-axis hinge type cubic press, and performing heating and pressurizing sintering, wherein the set pressure is 0.6-2.0GPa, the set temperature is 300-600 ℃ and the reaction time is 30-120 min.
The high-pressure assembly blockThe preparation and access method of the inner thermocouple comprises the following steps:
preparing a thermocouple: inserting the nickel-chromium wire and the nickel-silicon wire into the double-hole ceramic tube respectively, welding in a saturated sodium chloride solution with the voltage of 80-200V, and when the connection part of the nickel-chromium wire and the nickel-silicon wire is welded into a smooth small ball shape, the thermocouple is successfully prepared;
the thermocouple access method comprises the following steps: a small hole is drilled in the middle of the side edge of the pyrophyllite square block, a thermocouple is connected into the small hole, and the thermocouple is next to the boron nitride cylinder.
The sintered sample in the step 7 can be prepared into a high-purity compact arsenopyrite electrode, which means that the sintered sample can be prepared into electrodes with various shapes and meeting various experimental requirements by methods of mechanical cutting, grinding, polishing and the like.
Example 1:
crushing ore containing toxic placer into 40-80 meshes, and selecting the toxic placer with the purity of more than 98% under a binocular microscope. Ultrasonically cleaning with anhydrous ethanol for 10-20min, taking out, cleaning with anhydrous ethanol, and oven drying in a vacuum oven at 50 deg.C. Adding the weighed arsenopyrite powder into a powder tabletting cylindrical die, compacting for 2min in a powder tabletting machine under the condition of 0.5MPa, reversing the die, taking out the arsenopyrite cylinder, and wrapping with a silver foil. And pressing the arsenopyrite cylinder wrapped by the silver foil into a hole of the boron nitride cylinder, and covering the upper end and the lower end of the boron nitride cylinder with boron nitride wafers with the thickness of 3-5 mm. Putting the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil into the pyrophyllite block for high-pressure assembly. The specific assembling operation process comprises the following steps:
The size of the high-voltage assembly block can be specifically determined according to the requirements of the arsenopyrite electrode; in the assembly block, pyrophyllite and boron nitride are used as pressure transmission media, a stainless steel sheet is used as a heating furnace, and a nickel-chromium-nickel-silicon thermocouple is used as a temperature control device. The high-pressure assembly block has the advantages that: the pyrophyllite serving as a primary pressure transmission medium has good pressure transmission performance, machinability, heat resistance and heat preservation performance and insulativity, and boron nitride has excellent performances such as high hardness, good heat conductivity and the like and can provide a proper growth environment for a high-pressure synthesis process; two layers of stainless steel are used as a heating furnace, so that the cost is reduced, and the temperature can be ensured to be uniform. The temperature control of the nickel-chromium-nickel-silicon thermocouple has the advantages that: the linearity of the thermoelectromotive force is good; good oxidation resistance and stability in the temperature range set by the experiment. And after the high-pressure assembly block is finished, putting the high-pressure assembly block into a DS-6 x 1400t six-axis hinge type cubic press for heating, pressurizing and sintering, wherein the set pressure is 0.6 GPa, the set temperature is 300 ℃, the reaction time is 30min, and after the reaction is finished, taking out a sample to obtain the arsenopyrite cylinder with the purity of more than 98% and the relative density of 6.0-6.2. The arsenopyrite cylinder can be prepared into electrodes with various shapes and meeting various experimental requirements by methods of mechanical cutting, grinding, polishing and the like.
Example 2:
crushing ore containing toxic placer into 40-80 meshes, and selecting the toxic placer with the purity of more than 98% under a binocular microscope. Ultrasonically cleaning with anhydrous ethanol for 10-20min, taking out, cleaning with anhydrous ethanol, and oven drying in a vacuum oven at 50 deg.C. Adding the weighed arsenopyrite powder into a powder tabletting cylindrical die, compacting for 2min in a powder tabletting machine under the condition of 0.5MPa, reversing the die, taking out the arsenopyrite cylinder, and wrapping with a silver foil. And pressing the arsenopyrite cylinder wrapped by the silver foil into a hole of the boron nitride cylinder, and covering the upper end and the lower end of the boron nitride cylinder with boron nitride wafers with the thickness of 3-5 mm. Putting the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil into the pyrophyllite block for high-pressure assembly. The specific assembling operation process comprises the following steps:
The size of the high-voltage assembly block can be specifically determined according to the requirements of the arsenopyrite electrode; in the assembly block, pyrophyllite and boron nitride are used as pressure transmission media, a stainless steel sheet is used as a heating furnace, and a nickel-chromium-nickel-silicon thermocouple is used as a temperature control device. The high-pressure assembly block has the advantages that: the pyrophyllite serving as a primary pressure transmission medium has good pressure transmission performance, machinability, heat resistance and heat preservation performance and insulativity, and boron nitride has excellent performances such as high hardness, good heat conductivity and the like and can provide a proper growth environment for a high-pressure synthesis process; two layers of stainless steel are used as a heating furnace, so that the cost is reduced, and the temperature can be ensured to be uniform. The temperature control of the nickel-chromium-nickel-silicon thermocouple has the advantages that: the linearity of the thermoelectromotive force is good; good oxidation resistance and stability in the temperature range set by the experiment. And after the high-pressure assembly block is finished, putting the high-pressure assembly block into a DS-6 x 1400t six-axis hinge type cubic press for heating, pressurizing and sintering, wherein the set pressure is 1.0GPa, the set temperature is 400 ℃, the reaction time is 80min, and after the reaction is finished, taking out a sample to obtain the arsenopyrite cylinder with the purity of more than 98% and the relative density of 6.0-6.2. The arsenopyrite cylinder can be prepared into electrodes with various shapes and meeting various experimental requirements by methods of mechanical cutting, grinding, polishing and the like.
Example 3:
crushing ore containing toxic placer into 40-80 meshes, and selecting the toxic placer with the purity of more than 98% under a binocular microscope. Ultrasonically cleaning with anhydrous ethanol for 10-20min, taking out, cleaning with anhydrous ethanol, and oven drying in a vacuum oven at 50 deg.C. Adding the weighed arsenopyrite powder into a powder tabletting cylindrical die, compacting for 2min in a powder tabletting machine under the condition of 0.5MPa, reversing the die, taking out the arsenopyrite cylinder, and wrapping with a silver foil. And pressing the arsenopyrite cylinder wrapped by the silver foil into a hole of the boron nitride cylinder, and covering the upper end and the lower end of the boron nitride cylinder with boron nitride wafers with the thickness of 3-5 mm. Putting the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil into the pyrophyllite block for high-pressure assembly. The specific assembling operation process comprises the following steps:
The size of the high-voltage assembly block can be specifically determined according to the requirements of the arsenopyrite electrode; in the assembly block, pyrophyllite and boron nitride are used as pressure transmission media, a stainless steel sheet is used as a heating furnace, and a nickel-chromium-nickel-silicon thermocouple is used as a temperature control device. The high-pressure assembly block has the advantages that: the pyrophyllite serving as a primary pressure transmission medium has good pressure transmission performance, machinability, heat resistance and heat preservation performance and insulativity, and boron nitride has excellent performances such as high hardness, good heat conductivity and the like and can provide a proper growth environment for a high-pressure synthesis process; two layers of stainless steel are used as a heating furnace, so that the cost is reduced, and the temperature can be ensured to be uniform. The temperature control of the nickel-chromium-nickel-silicon thermocouple has the advantages that: the linearity of the thermoelectromotive force is good; good oxidation resistance and stability in the temperature range set by the experiment. And after the high-pressure assembly block is finished, putting the high-pressure assembly block into a DS-6 x 1400t six-axis hinge type cubic press for heating, pressurizing and sintering, wherein the set pressure is 2.0GPa, the set temperature is 600 ℃, the reaction time is 120min, and after the reaction is finished, taking out a sample to obtain the arsenopyrite cylinder with the purity of more than 98% and the relative density of 6.0-6.2. The arsenopyrite cylinder can be prepared into electrodes with various shapes and meeting various experimental requirements by methods of mechanical cutting, grinding, polishing and the like.
Claims (4)
1. A preparation method of a high-purity compact arsenopyrite electrode comprises the following steps:
step 1, selecting arsenopyrite particles;
step 2, cleaning and drying the selected arsenopyrite particles for later use; the method for drying the washed arsenopyrite particles in the step 2 comprises the following steps: ultrasonically cleaning with anhydrous ethanol for 10-20min, taking out, cleaning with anhydrous ethanol, and oven drying at 50 deg.C in a vacuum oven;
step 3, grinding the dried arsenopyrite into powder with the granularity of more than 200 meshes, weighing 0.8-1.0g of arsenopyrite powder, pressing the arsenopyrite powder into a arsenopyrite cylinder in a powder tablet press, and wrapping the arsenopyrite cylinder by using a silver foil;
step 4, pressing the silver foil wrapped arsenopyrite cylinder into boron nitride to prepare a boron nitride cylinder containing the silver foil wrapped arsenopyrite cylinder;
step 5, putting the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil into a pyrophyllite block for high-pressure assembly;
step 5, the method for putting the pyrophyllite block into the high-pressure assembling machine comprises the following steps:
step 5.1, selecting a pyrophyllite square block, and drilling a circular through hole in the center of the pyrophyllite block;
step 5.2, placing a circular stainless steel heating sheet on the inner wall of the through hole;
step 5.3, placing a boron nitride cylinder containing a silver foil wrapped arsenopyrite cylinder in the middle of the stainless steel heating plate, and sealing and compacting the upper end and the lower end by a pyrophyllite plug;
step 5.4, connecting a thermocouple into the pyrophyllite square block;
the access method of the thermocouple comprises the following steps:
preparing a thermocouple: respectively inserting a nickel-chromium wire and a nickel-silicon wire into the double-hole ceramic tube, and welding in a saturated sodium chloride solution with the voltage of 80-200V;
thermocouple access: drilling a hole in the middle of a side edge of a pyrophyllite square block, and connecting a thermocouple into the hole, wherein the thermocouple is close to a boron nitride cylinder;
step 6, heating, pressurizing and sintering in a large-cavity press;
the method for heating and pressurizing sintering by the large-cavity press in the step 6 comprises the following steps: assembling pyrophyllite blocks under high pressure, placing the pyrophyllite blocks into a six-axis hinge type cubic press, heating, pressurizing and sintering, wherein the pressure is 0.6-2.0GPa, the temperature is 300-600 ℃, and the reaction time is 30-120 min;
and 7, stripping silver foil on the surface of the sintered sample to prepare the high-purity compact arsenopyrite electrode.
2. The method for preparing the high-purity compact arsenopyrite electrode according to claim 1, wherein the method comprises the following steps: the method for selecting the arsenopyrite particles in the step 1 comprises the following steps: crushing ore containing toxic placer into 40-80 meshes, and selecting the toxic placer with the purity of more than 98% under a binocular microscope.
3. The method for preparing the high-purity compact arsenopyrite electrode according to claim 1, wherein the method comprises the following steps: the method for preparing the arsenopyrite cylinder in the step 3 comprises the following steps: adding the weighed arsenopyrite powder into a powder tabletting cylindrical die, compacting for 2min in a powder tabletting machine under the condition of 0.5MPa, reversing the die, taking out the arsenopyrite cylinder, and wrapping with a silver foil.
4. The method for preparing the high-purity compact arsenopyrite electrode according to claim 1, wherein the method comprises the following steps: the method for preparing the boron nitride cylinder containing the arsenopyrite cylinder wrapped by the silver foil comprises the following steps: processing boron nitride into a rod shape, cutting a boron nitride cylinder with the same length as the arsenopyrite cylinder, drilling a hole with the same diameter as the arsenopyrite cylinder wrapped by the silver foil on the boron nitride cylinder, pressing the arsenopyrite cylinder wrapped by the silver foil into the hole of the boron nitride cylinder, and covering boron nitride wafers with the thickness of 3-5mm at the upper end and the lower end of the boron nitride cylinder.
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