TWI523044B - Processing solution for producing magnetic iron powder and its recovery method - Google Patents

Description

Processing solution for manufacturing magnetic iron powder and recycling method thereof

The invention relates to a treatment solution and a recovery method thereof, in particular to preparing a treatment solution, and then changing with a magnetic iron powder (such as secondary reduced iron powder or carbonyl iron powder or iron chrome iron powder) through a manufacturing process to manufacture The surface is formed with a layer of insulating pressure and high temperature resistant film, and at the same time, the processing solution is recycled and reused in the manufacturing process.

In the prior art, in the process of performing surface insulation of magnetic iron powder (such as secondary reduced iron powder or carbonyl iron powder or iron ferrochrome powder), phosphoric acid and solvent are added in sequence to the process (ie, phosphating). And the magnetic iron powder is stirred and dried until it is passed through a stirrer, and then the second stage is added to the solvent (that is, esterification) with phenolphthalein, and the mixture is stirred until the dryness is 70%, and then the magnetic iron is further applied. Powder granulation, in order to facilitate the future production of the feed and increase the fluidity of the magnetic iron powder.

As described above, in the treatment process of phosphating and esterification, a secondary treatment process is required, and the secondary treatment process takes 4 to 5 hours, and the treatment process is rather cumbersome and requires baking. 160 ° C to 180 ° C and more than 2 hours to allow the solvent to volatilize in the air, this practice, not only very environmentally friendly, but also easy to cause gas explosion, and will also cause damage to the health of workers.

Furthermore, the magnetic iron powder formed by the prior art has the problems that the iron powder is easily aggregated, the surface phosphating insulation is incomplete, the phenolphthalein is used too much, and the insulation is poor, and the quality is not optimal. For the purpose of the invention, the technology of the present invention has been proposed.

An object of the present invention is to provide a treatment solution for manufacturing magnetic iron powder, which can complete the treatment process of phosphating and esterification in one time by preparing the treatment solution, thereby effectively reducing the time required for the conventional treatment process (the present invention) One-time process takes only 40 minutes) and baking temperature and time (The baking temperature and time of the invention only need 160 ° C and 1 hour), in order to achieve rapid manufacturing and energy saving; the magnetic iron powder formed by the invention (such as: secondary reduced iron powder or carbonyl iron powder or iron) The surface treatment of ferrochrome powder can achieve a uniform coating of a thin liquid glass insulating layer on the surface, less use of insulating materials, high magnetic permeability (μi), good insulation, and low eddy current loss (Eddy loss). The optimum quality of high temperature resistant film.

The technical means for achieving the above object of the present invention is to prepare a treatment solution comprising a liquid glass (phosphoric acid and cerium oxide solate), an epoxy resin and an acetone solvent, wherein the liquid is composed. The glass blending ratio is 20%, the epoxy resin blending ratio is 40%, and the acetone solvent blending ratio is 40%, and the liquid glass (phosphoric acid and cerium oxide dissolved matter), epoxy resin, and acetone The solvent ratio is determined according to the selected magnetic iron powder (such as: secondary reduced iron powder or carbonyl iron powder or iron ferrochrome powder) and the weight; and the liquid glass is prepared by adding cerium oxide powder. 30% to 40%, phosphoric acid 60% to 70%, and heating at 120 ° C to 200 ° C to stir until the cerium oxide powder dissolves to a transparent or light yellow transparent.

Another object of the present invention is to provide a method for recovering a treatment solution for producing magnetic iron powder by using the treatment solution and magnetic iron powder (for example, secondary reduced iron powder or carbonyl iron powder or iron ferrochrome powder) in a treatment process The reaction can be recycled and reused at the same time to achieve environmental protection, safety and energy conservation.

The technical means for achieving the other object of the present invention is as follows: when a magnetic iron powder to be treated (for example, secondary reduced iron powder or carbonyl iron powder or iron ferrochrome powder) is placed in a stirred tank of a mixer, At the same time, the prepared treatment solution is placed therein, and the treatment solution and the magnetic iron powder are uniformly stirred by stirring; then, the treatment solution and the magnetic iron are pulverized and heated by a pulverizing motor in the mixer. The powders are combined with each other and completed; that is, granulated by a pellet granulator according to the desired number of granules; then dried in an oven; sieved through a vibrating screen machine, and sampled by a molding machine; The sample is then baked in an oven and tested by a pressure tester; finally, the qualified magnetic iron powder is stored in a vacuum packaging machine.

As described above, the method for recovering the treatment solution of the present invention is to separately recover the treatment solution by distillation in a process in which the treatment solution and the magnetic iron powder are combined and reacted, and then use a gas chromatograph (Gas Chromatography). Used to detect and analyze the treatment The liquid purity, and a moisture meter are used to detect and analyze the amount of ppm of the treatment solution, and then the treatment solution can be prepared according to the ratio of the ppm content to achieve repeated recycling and reuse.

Please refer to the following detailed description of a preferred embodiment of the present invention and the accompanying drawings, which will further understand the technical content of the present invention and its effect:

Fig. 1 is a flow chart showing the recovery of the treatment solution of the present invention applied to the manufacturing process of magnetic iron powder.

The invention provides a treatment solution for manufacturing magnetic iron powder, which is prepared by a process of the preparation of the treatment solution and a magnetic iron powder (such as: secondary reduced iron powder or carbonyl iron powder or iron ferrochrome powder). The surface of the magnetic iron powder is formed with a layer of insulating withstand voltage and high temperature resistant film; the treatment solution of the invention comprises a liquid glass (phosphoric acid and cerium oxide dissolved matter), an epoxy resin and an acetone solvent. The liquid glass composition ratio is 20%, the epoxy resin compounding ratio is 40%, and the acetone solvent compounding ratio is 40%, and the liquid glass (phosphoric acid and cerium oxide solute) The ratio of the epoxy resin to the acetone solvent is determined according to the selected different magnetic iron powder and its weight; and the liquid glass is prepared by adding cerium oxide powder 30% to 40%, phosphoric acid 60. From 100% to 70%, the mixture is heated at 120 ° C to 200 ° C until the cerium oxide powder dissolves to a transparent or light yellow transparent.

Referring to FIG. 1 , a manufacturing step of forming a layer of insulating withstand voltage and high temperature resistant film on the surface of the magnetic iron powder for treating the solution and the magnetic iron powder: Step (101): a magnetic to be processed and scaled Iron powder (such as: secondary reduced iron powder or carbonyl iron powder or iron ferrochrome powder 10 kg) is placed in a stirred tank of a mixer (rotation speed of about 20 rev / min); step (102): will be handled well The solution is placed in the agitation tank described above, and the treatment solution and the magnetic iron powder are uniformly stirred by stirring (the rotation speed is increased to 90 rpm and the stirring is stopped for 20 seconds to allow the iron powder to be sufficiently reacted); Step (103): The pulverized motor in the mixer is pulverized and heated (temperature is 70 to 140 degrees), so that the treatment solution and the magnetic iron powder are bonded to each other to dryness (about 7 minutes). Dry) and the reaction is completed; step (104): granulation by a pellet granulator according to the desired number of granules; step (105): baking into an oven (100 degree baking for 1 hour); step (106) ): sieved through a vibrating screen machine, and sampled by a molding machine; step (107): the sample is baked in the oven (140 degree baking for 2 hours), and the sample is tested by a pressure tester; Step (108): finally, the qualified magnetic iron powder is stored in a vacuum packaging machine, and the step (109) is characterized in that the method for recovering the processing solution for manufacturing the magnetic iron powder provided by the present invention is in the step (103) When the treatment solution and the magnetic iron powder are bonded to each other to a process of drying and reacting, the treatment solution is separately recovered by distillation, and then gas chromatograph (Gas Chromatography) is used for detection and analysis. The purity of the treatment solution, and a moisture meter for detecting and analyzing the amount of ppm of the treatment solution, and then formulating the treatment solution according to the ratio of the ppm content can be repeatedly recycled and reused.

According to the surface treatment of the magnetic iron powder formed by the foregoing steps, a thin liquid glass insulating layer can be uniformly coated on the surface, the insulating material is used less, the magnetic permeability (μi) is high, the insulation is good, and the Eddy loss is small. The optimum quality of the insulation withstand voltage and high temperature resistant film.

As described above, the ratio of the liquid glass (phosphoric acid and cerium oxide dissolved matter), epoxy resin and acetone solvent is determined according to the different magnetic iron powders selected and their weights. Therefore, it should be noted that When the magnetic iron powder is applied to an inductor in the future, the thickness of the liquid glass combined with the epoxy resin coated on the surface of the magnetic iron powder affects the magnetic permeability (μi) of the inductor and reduces the amount of use. The magnetic permeability (μi) will become higher, and the magnetic permeability (μi) will decrease when the usage is increased; however, the magnetic permeability (μi) will become higher when the liquid glass is used less, and the magnetic permeability will be increased when the usage is increased. The rate (μi) is lowered. Therefore, the mixing ratio and the steps of the liquid glass combined with the epoxy resin need to be strictly controlled and the control is strict.

Further, since the cerium oxide powder is generally incapable of dissolving, only phosphoric acid can be dissolved, and the use thereof is to produce a glass protective film on the surface of the inductor, which can increase the oxidation time; The glass-bonded epoxy resin is mixed with an acetone solvent, and the magnetic iron powder is used to form each iron powder, which is mutually co-dissolved. If the ratio is not correct, it cannot be reacted and the iron powder can not be dried. The overall process needs to maintain the three principles of quantification, constant temperature and timing. The process can be safe and the quality can be optimized.

It is further explained that when the magnetic iron powder is applied to the inductor in the future, the most important thing in the production of the inductor is that the high temperature sintering does not cause cracking, especially when the heat source in the oven is unevenly generated, and cracking occurs. The rate is generated from the majority, and the treatment solution prepared by the present invention has overcome this phenomenon. In addition, an iron powder dispenser is required at the molding end, and the advantages are: high average, uniform weight and average inductance, and the yield can reach 95% or more, which is used to improve the defect rate problem.

The detailed description above is a detailed description of a possible embodiment of the present invention, and is not intended to limit the scope of the present invention, and equivalents and modifications, such as variations, etc., without departing from the spirit of the invention. Equivalent embodiments are to be included in the scope of the patent.

Claims (4)

A processing solution for manufacturing a magnetic iron powder, comprising: a liquid glass (phosphoric acid and cerium oxide solute), an epoxy resin and an acetone solvent, wherein the liquid glass is formulated at a ratio of 20%, The blending ratio of the epoxy resin was 40% and the blending ratio of the acetone solvent was 40%. The processing solution for manufacturing magnetic iron powder according to claim 1, wherein the liquid glass is prepared by adding cerium oxide powder 30% to 40%, phosphoric acid 60% to 70%, and heating 120 ° C to Stir at 200 ° C until the ceria powder dissolves to a clear or light yellow transparent. A method for recovering a treatment solution for producing magnetic iron powder according to claim 1 of the patent application, in particular, the treatment solution and a magnetic iron powder are subjected to the following manufacturing steps to form an insulating withstand voltage on the surface thereof. And the high temperature resistant film: the magnetic iron powder to be processed and weighed is placed in a stirring tank of a mixer; the prepared treatment solution is placed in the stirring tank, and the processing solution and the magnetic iron powder are stirred and stirred. Uniformly; pulverized and heated by a pulverizing motor in the mixer, the treatment solution and the magnetic iron powder are combined with each other to dry and the reaction is completed; granulation is carried out by a particle granulator according to the desired number of granules; The oven is baked and dried; it is sieved by a vibrating screen machine, and sampled by a molding machine; the sample is baked in an oven and tested by a pressure tester; finally, the qualified magnetic iron powder is vacuumed. The packaging machine is packaged and stored; the method is characterized in that the recycling method is a process in which the treatment solution and the magnetic iron powder are combined to dry and the reaction is completed, and the distillation method is performed. The treatment solution is separately recovered, and a gas chromatograph is used to detect and analyze the purity of the treatment solution, and a moisture meter is used to detect and analyze the amount of ppm of the treatment solution, and then the ratio is adjusted according to the ratio of the ppm content. The solution is treated to achieve repeated recycling and reuse. The method for recovering a treatment solution for producing magnetic iron powder according to claim 3, wherein the magnetic iron powder is one selected from the group consisting of secondary reduced iron powder, carbonyl iron powder, and iron ferrochrome powder.