RU2241053C1 - Method for producing of copper phosphide powder - Google Patents

Abstract

FIELD: non-iron metallurgy, in particular manufacturing of addition alloy, modifier, solder alloy and past.

SUBSTANCE: Claimed method includes preparation of batch by mixing of copper particles and red phosphorous powder, heating, conditioning and cooling, while batch in reactor is continuously mixed. Heating, conditioning and cooling are carried out in moving closed reactor in the presence of grinding bodies. Temperature of heating and conditioning is lower than eutectic temperature in copper-phosphorous system (namely of 714⁰C).

EFFECT: reduced cost for producing of copper phosphide and environmental acceptability.

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Description

The invention relates to ferrous metallurgy, in particular to methods for producing phosphorous copper used for the production of alloys, deoxidants, modifiers and solders.

The purpose of the invention: increasing the speed of the process by reducing diffusion difficulties in the process of producing phosphides, reducing phosphorus losses.

This goal is achieved by the fact that in the known method for producing a copper-phosphorous ligature, which includes preparing the charge by mixing copper particles and red phosphorus powder, followed by heating, holding and cooling with continuous movement of the charge, obtaining copper-phosphorus ligature powder is carried out in a moving closed reactor in the presence of grinding media at temperatures below the eutectic transformation temperature in the copper - phosphorus system equal to 714 ° С.

The copper phosphide layer formed in the process of obtaining powder on copper particles contains up to 30 percent or more of phosphorus [1] and impedes the access of phosphorus vapor to copper particles. The mechanical removal of this layer by the mechanical action of grinding media increases the rate of phosphide formation by more than 3 times.

A known method for producing copper-phosphorous ligatures, including the simultaneous loading of copper scrap with a developed reaction surface (shavings) and red phosphorus into a ceramic crucible, isolation of the crucible from the environment, holding the crucible in an oven at temperatures of 350-360 ° C for 4-5 hours followed by cooling. The powder is obtained by crushing and grinding any ligature [2].

The disadvantages of the method include: high energy consumption, significant (up to 10%) loss of phosphorus in the furnace atmosphere and the associated costs of cleaning the exhaust gases to sanitary standards, the need for crushing and grinding cake to obtain powder.

As a prototype, a method for producing a copper-phosphorous ligature was selected, according to which a mixture is prepared by mixing copper particles, for example, crushed current conductors (granules or shavings), and red phosphorus powder by alternating layers of copper particles with a specific surface area of 0.1-1.0 sq. m / kg and phosphorus at a ratio of 9: (1-4), then the mixture is subjected to heat treatment at temperatures of 370-420 ° C for 30-90 minutes, followed by cooling with continuous movement of the reaction mass [3].

The disadvantages of the method include the low rate of production of copper phosphide, the possibility of breakthrough of phosphorus vapor from the reaction zone to the atmosphere through layers of particles of copper and red phosphorus powder, which may occur during synthesis due to the high vapor pressure of phosphorus (at a temperature of 420 ° C) reaches the 1st atmosphere in violation of technological regimes.

The following are examples of the implementation of the proposed method in the factory.

Example 1

A sample of chopped into pieces 5-15 cm long copper scrap (cable core, wire) weighing 80 kg, 20 kg of red phosphorus and grinding media in an amount of 20 kg was placed in a cylindrical container, the feed opening was sealed and heated at a rate of 200 ° C in hour while rotating the container. After this, the rotation of the tank was interrupted, the gas pressure in the cavity of the tank was reduced to atmospheric by opening the bleed valve. Then the valve was closed, the container was again rotated with simultaneous heating to a temperature of 700 ° C and kept at this temperature for 5 hours. Then the container, without stopping rotation, was forcedly cooled to ambient temperature and the powder was unloaded. The powder contained 20% phosphorus.

Example 2

In the conditions of example 1, 70 kg of chopped copper scrap-cable strand, red phosphorus in the amount of 30 kg and 20 kg of grinding media (stainless steel rods) were placed in a cylindrical container, the container was rotated with simultaneous heating to a temperature of 714 ° C and kept at this temperature for 7 hours. Then the rotation and heating were stopped, and the container was forcibly cooled to ambient temperature. The phosphorus content in the powder was 30%; the powder contained 10% cakes in the form of balls with a diameter of 10-30 mm.

Example 3

Under the conditions of Example 2, 70 kg of chopped scrap of electrical copper cable core 30 kg of red phosphorus were placed in a cylindrical container, grinding media were not loaded into the container. Heating and rotation were carried out to a temperature of 720 ° C for 10 hours. Then, without stopping rotation, the container was forcibly cooled to ambient temperature and copper phosphide powder, which contained 30% phosphorus, was unloaded. At the same time, during the synthesis of phosphide, 20% spherical specimens were formed in the container and the fused with the walls of the retort were accustomed.

Example 4

In the conditions of example 2, the tank was heated to a temperature of 500 ° C and kept with simultaneous rotation for 10 hours. After cooling and unloading from the tank, free phosphorus was contained in the powder (the obtained powder ignited from a match flame).

Example 5

In the conditions of example 2, the tank was heated to 500 ° C, kept with simultaneous rotation for 12 hours. The finished product - phosphorous copper powder from the match flame did not ignite, i.e. did not contain free phosphorus. The content of “bound” phosphorus in the finished product is 30%.

Example 6

In the conditions of example 2, the tank was heated to a temperature of 720 ° C and kept with simultaneous rotation for 12 hours. After cooling, the composition of the finished product - powder contained large specimen balls up to 30 mm in size, which reduced the yield of the powder to 85%.

The table shows the conditions and results of the powder of the copper-phosphorus ligature in comparison with the prototype method.

Sources of information

1. Radzikhovsky V.A., Vorobyov A.K. Research report, topic 26-89P-14 “To find rational and environmentally friendly technologies for producing high phosphorous ligatures”. - Donetsk, 1990

2. Kurdyumov A.V., Pikunov M.V., Chursin V.M. "Foundry of non-ferrous metals." - M.: Metallurgy, p. 188.

3. Copyright certificate SU No. 1788059, cl. C 22 C 1 / 2.9 / 00.

Claims (1)

A method of producing copper phosphide powder, including preparing the charge by mixing copper particles and red phosphorus powder, heating, holding and cooling with continuous movement of the charge in the reactor, characterized in that to reduce the cost of producing copper phosphide powder, eliminating phosphorus loss to the environment, heating, aging and cooling during continuous movement of the charge is carried out in a moving closed reactor in the presence of grinding media, and heating and aging are carried out at a temperature below the eutectic temperature in the copper - phosphorus system, equal to 714 ° С.