Composite solid additive for silicon steel and preparation method thereof

By preparing composite solid additives with finer and more uniform particle size, the problems of particle size and element distribution in silicon steel production of traditional additives have been solved, simplifying the operation process and improving product performance. In particular, the addition of CaO enhances the coating and adhesion properties of magnesium oxide.

CN116555542BActive Publication Date: 2026-03-27SHANGHAI SIIC ZHENTAI CHEM CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-04-27
Publication Date
2026-03-27

AI Technical Summary

Technical Problem

Traditional solid additives have problems in silicon steel production, such as uneven particle size, uneven element distribution, cumbersome operation, and harsh storage conditions, making it difficult to meet the strict requirements of high magnetic induction oriented silicon steel production.

Method used

A composite solid additive containing titanium, boron, antimony, strontium, calcium and active MgO is used. By uniformly mixing and calcining at a specific temperature and pulverizing, an additive with finer and more uniform particle size is prepared, which simplifies the operation process and improves the fusion effect of elements.

Benefits of technology

It achieves better dispersibility and mixability of additives, simplifies operation procedures, reduces production costs, and improves the performance and quality of silicon steel products. In particular, the addition of CaO enhances the coating and adhesion properties of magnesium oxide.

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Abstract

The application discloses a kind of composite solid additives for silicon steel, its composition is: titanium 500-1500ppm, boron 500-1500ppm, antimony 500-1500ppm, strontium 800-1500ppm, calcium 500-1000ppm, sulfate radical 800-1500ppm, the rest is active MgO.The particle size of the composite solid additives for silicon steel of the application is uniform, the dispersibility is better, it is easy to use, simple to prepare, energy consumption is less, yield is high, and production cost is low;In addition, it can also enhance the coating property of magnesium oxide slurry, increase the reaction capacity of magnesium silicate bottom layer.
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Description

Technical Field

[0001] This invention relates to the field of metallurgy and chemical engineering, and in particular to a composite solid additive for silicon steel and its preparation method. Background Technology

[0002] Oriented silicon steel sheets are a type of cold-rolled silicon steel, possessing advantages such as high electromagnetic strength and low electrical loss, and belong to the category of special electrical steels. Magnesium oxide is commonly used in the production of oriented silicon steel sheets as a high-temperature annealing release agent and a material for forming the forsterite coating. Currently, the production of high-magnetic-induction oriented silicon steel (HiB) in China is becoming increasingly large-scale and rapid, leading to increasingly stringent requirements for magnesium oxide release agents. Simultaneously, to ensure the magnesium silicate underlayer grows in a specific direction and improves product performance and quality, other additives are needed to add certain trace elements. Currently, the additives used domestically are still traditional solid additives developed independently decades ago. However, with the advancement of silicon steel production technology, the requirements for raw materials are becoming increasingly stringent, and traditional solid additives are encountering various problems, such as particle size issues, uneven element distribution, the need for specific element replenishment, cumbersome types, and demanding storage conditions.

[0003] Therefore, based on the current situation and needs, it is necessary to upgrade traditional solid additives and redesign and develop a new type of composite solid additive. Summary of the Invention

[0004] The purpose of this invention is to provide a composite solid additive for silicon steel and its preparation method to solve the above-mentioned problems.

[0005] The technical solution adopted in this invention is as follows:

[0006] A composite solid additive for silicon steel comprises: titanium 500-1500 ppm, boron 500-1500 ppm, antimony 500-1500 ppm, strontium 800-1500 ppm, calcium 500-1000 ppm, sulfate 800-1500 ppm, and the remainder being active MgO. The preparation method of the above-mentioned composite solid additive for silicon steel is as follows:

[0007] (1) Weigh 10-20 parts of pure water into a stainless steel container and stir continuously;

[0008] (2) Weigh out SbCl3 solid according to the antimony content in the composite solid additive for silicon steel being 500-1500ppm, slowly add it to the pure water in step (1), and stir continuously for 10-15 minutes until uniform.

[0009] (3) Weigh out TiO2 powder according to the ratio of titanium content in composite solid additives for silicon steel of 500-1500ppm, add it to the slurry obtained in step (2), and stir continuously for 5-10 minutes until uniform.

[0010] (4) Weigh out H3BO3 solid according to the ratio of boron content in composite solid additives for silicon steel of 500-1500ppm, add it to the slurry obtained in step (3), and stir continuously for 5-10 minutes until uniform.

[0011] (5) Weigh out SrCO3 powder according to the ratio of 800-1500ppm strontium content in the composite solid additive for silicon steel, add it to the slurry obtained in step (4), and stir continuously for 5-10 minutes until uniform;

[0012] (6) Weigh out CaSO4 solid according to the ratio of 500-1000ppm calcium content in the composite solid additive for silicon steel, add it to the slurry obtained in step (5), and stir continuously for 5-10 minutes until uniform.

[0013] (7) Weigh 5-10 parts of active MgO by mass, add it to the slurry obtained in step (6), and heat and stir at 40°C for 10-20 minutes;

[0014] (8) Dry the slurry prepared in step (7) at 120~200℃;

[0015] (9) Place the solid obtained in step (8) in a high-temperature resistant container and calcine it at 400~500℃ for 2~3 hours;

[0016] (10) The solid obtained in step (9) is crushed and ground until the particle size D50≤3um to obtain the composite solid additive for silicon steel.

[0017] The composite solid additive for silicon steel of the present invention has the following advantages over traditional solid additives:

[0018] (1) The particle size is finer and more uniform, and the dispersion is better when it is stirred together with silicon steel magnesium oxide, so that it can be fully mixed and the effect is better;

[0019] (2) It can combine the required components and trace elements together in one operation, reducing the number of operation steps for customers. It is easy to use and can ensure that all components can be added and mixed at the same time, making the effect more obvious.

[0020] (3) The preparation process is simple, with few reaction steps, low energy consumption, and high yield;

[0021] (4) Compared with traditional solid additives that are individually pulverized in batches and then mixed, the new composite solid additives are mixed and reacted in one step before pulverization, which reduces processing steps and production costs.

[0022] (5) The addition of calcium enhances the coatability of magnesium oxide slurry and helps improve the performance of silicon steel products. Calcium exists as solid CaO in the solid additive. The reaction between CaO and H2O is vigorous and exothermic, which promotes the combination of other elements with water and MgO during stirring. Furthermore, the produced Ca(OH)2 is a binder with good adhesion, improving the adhesion performance of magnesium oxide on silicon steel. The main reaction involved is CaO + H2O → Ca(OH)2.

[0023] (6) The hydration of active magnesium oxide to generate magnesium hydroxide can effectively encapsulate and fused other elements together. Calcination does not affect the elemental composition or the activity of magnesium oxide, and increases the reactivity of the magnesium silicate substrate. Within a reasonable range, for every 500 ppm increase in Ca content, the grade of silicon steel sheet will increase by approximately 0.5 grades, and the iron loss will decrease by about 0.1%.

[0024] (7) It is convenient and feasible to add corresponding elements and components in the subsequent process according to application needs and customer requirements; Detailed Implementation

[0025] The preferred embodiments of the present invention are given below to illustrate the technical solution of the present invention in detail.

[0026] Example 1

[0027] (1) Weigh 10 portions of pure water into a stainless steel container and stir continuously;

[0028] (2) Weigh out SbCl3 solid according to the antimony content of 500ppm, slowly add it to the pure water in step (1), and stir continuously for 10min until uniform;

[0029] (3) Weigh out TiO2 powder at a titanium content of 500 ppm, add it to the slurry obtained in step (2), and stir continuously for 5 minutes until uniform;

[0030] (4) Weigh out H3BO3 solid at a boron content of 500ppm, add it to the slurry obtained in step (3), and stir continuously for 5 minutes until uniform;

[0031] (5) Weigh out SrCO3 powder with a strontium content of 800 ppm, add it to the slurry obtained in step (4), and stir continuously for 5 minutes until uniform;

[0032] (6) Weigh out CaSO4 solid at a calcium content of 500 ppm, add it to the slurry obtained in step (5), and stir continuously for 5 minutes until uniform;

[0033] (7) Weigh 5 portions of active MgO by mass, add them to the slurry obtained in step (6), and heat and stir at 40°C for 10 min;

[0034] (8) Dry the slurry prepared in step (7) at 120°C;

[0035] (9) Place the solid obtained in step (8) in a high-temperature resistant container and calcine it at 400°C for 2 hours;

[0036] (10) The solid obtained in step (9) is crushed and ground until the particle size D50≤3um to obtain the composite solid additive for silicon steel.

[0037] Example 2

[0038] (1) Weigh 20 portions of pure water into a stainless steel container and stir continuously;

[0039] (2) Weigh out SbCl3 solid according to the antimony content of 1500ppm, slowly add it to the pure water in step (1), and stir continuously for 15 minutes until uniform;

[0040] (3) Weigh out TiO2 powder at a titanium content of 1500 ppm, add it to the slurry obtained in step (2), and stir continuously for 10 min until uniform;

[0041] (4) Weigh out H3BO3 solid at a boron content of 1500ppm, add it to the slurry obtained in step (3), and stir continuously for 10 minutes until uniform;

[0042] (5) Weigh out SrCO3 powder with a strontium content of 1500ppm, add it to the slurry obtained in step (4), and stir continuously for 10 minutes until uniform;

[0043] (6) Weigh out CaSO4 solid at a calcium content of 1000ppm, add it to the slurry obtained in step (5), and stir continuously for 10 minutes until uniform;

[0044] (7) Weigh 10 parts of active MgO by mass, add it to the slurry obtained in step (6), and heat and stir at 40°C for 20 minutes;

[0045] (8) Dry the slurry prepared in step (7) at 200°C;

[0046] (9) Place the solid obtained in step (8) in a high-temperature resistant container and calcine it at 500°C for 3 hours;

[0047] (10) The solid obtained in step (9) is crushed and ground until the particle size D50≤3um to obtain the composite solid additive for silicon steel.

[0048] Example 3

[0049] (1) Weigh 15 portions of pure water into a stainless steel container and stir continuously;

[0050] (2) Weigh out SbCl3 solid according to the antimony content of 1200ppm, slowly add it to the pure water in step (1), and stir continuously for 12 minutes until uniform;

[0051] (3) Weigh out TiO2 powder at a titanium content of 1200ppm, add it to the slurry obtained in step (2), and stir continuously for 10 minutes until uniform;

[0052] (4) Weigh out H3BO3 solid at a boron content of 1200ppm, add it to the slurry obtained in step (3), and stir continuously for 8 minutes until uniform;

[0053] (5) Weigh out SrCO3 powder at a ratio of 1200ppm strontium content, add it to the slurry obtained in step (4), and stir continuously for 8 minutes until uniform;

[0054] (6) Weigh out CaSO4 solid at a calcium content of 800 ppm, add it to the slurry obtained in step (5), and stir continuously for 8 minutes until uniform;

[0055] (7) Weigh 8 portions of active MgO by mass, add them to the slurry obtained in step (6), and heat and stir at 40°C for 16 minutes;

[0056] (8) Dry the slurry prepared in step (7) at 180°C;

[0057] (9) Place the solid obtained in step (8) in a high-temperature resistant container and calcine it at 500°C for 2.5 hours;

[0058] (10) The solid obtained in step (9) is crushed and ground until the particle size D50≤3um to obtain the composite solid additive for silicon steel.

[0059] Example 4

[0060] (1) Weigh 12 portions of pure water into a stainless steel container and stir continuously;

[0061] (2) Weigh out SbCl3 solid according to the antimony content of 1100ppm, slowly add it to the pure water in step (1), and stir continuously for 12 minutes until uniform;

[0062] (3) Weigh out TiO2 powder at a titanium content of 1100ppm, add it to the slurry obtained in step (2), and stir continuously for 10 minutes until uniform;

[0063] (4) Weigh out H3BO3 solid at a boron content of 1100ppm, add it to the slurry obtained in step (3), and stir continuously for 8 minutes until uniform;

[0064] (5) Weigh out SrCO3 powder at a ratio of 1100ppm strontium content, add it to the slurry obtained in step (4), and stir continuously for 8 minutes until uniform;

[0065] (6) Weigh out CaSO4 solid at a calcium content of 700 ppm, add it to the slurry obtained in step (5), and stir continuously for 8 minutes until uniform;

[0066] (7) Weigh 7 portions of active MgO by mass, add them to the slurry obtained in step (6), and heat and stir at 40°C for 15 minutes;

[0067] (8) Dry the slurry prepared in step (7) at 180°C;

[0068] (9) Place the solid obtained in step (8) in a high-temperature resistant container and calcine it at 500°C for 2.5 hours;

[0069] (10) The solid obtained in step (9) is crushed and ground until the particle size D50≤3um to obtain the composite solid additive for silicon steel.

[0070] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed invention.

Claims

1. A method for preparing a composite solid additive for silicon steel, characterized by, According to the following steps are prepared: (1) by mass 10-20 parts of pure water, stirring constantly; (2) according to the proportion of the content of antimony in the composite solid additive for silicon steel in 500-1500ppm SbCl3 solid, added to step (1) pure water, and constantly stirring 10-15 min to uniform; (3) according to the proportion of the content of titanium in the composite solid additive for silicon steel in 500-1500ppm TiO2 powder, added to step (2) obtained slurry, and constantly stirring 5-10 min to uniform; (4) according to the proportion of the content of boron in the composite solid additive for silicon steel in 500-1500ppm H3BO3 solid, added to step (3) obtained slurry, and constantly stirring 5-10 min to uniform; (5) according to the proportion of the content of strontium in the composite solid additive for silicon steel in 800-1500ppm SrCO3 powder, added to step (4) obtained slurry, and constantly stirring 5-10 min to uniform; (6) according to the proportion of the content of calcium in the composite solid additive for silicon steel in 500-1000ppm CaSO4 solid, added to step (5) obtained slurry, and constantly stirring 5-10 min to uniform; (7) according to the proportion of the content of calcium in the composite solid additive for silicon steel in 500-1000ppm CaSO4 solid, added to step (5) obtained slurry, and constantly stirring 5-10 min to uniform; (7) according to the proportion of the content of calcium in the composite solid additive for silicon steel in 500-1000ppm CaSO4 solid, added to step (5) obtained slurry, and constantly stirring 5-10 min to uniform; (8) the step (7) prepared slurry in 120-200 ℃ conditions under drying; (9) the step (8) obtained solid placed in a high temperature container, in 400-500 ℃ conditions calcined 2-3 h; 2. A composite solid-state additive for silicon steel, characterized by, (10) the step (9) obtained solid is ground to a particle size of D50≤3um, namely the composite solid additive for silicon steel. According to the method of claim 1 is prepared, the composition is: titanium 500-1500ppm, boron 500-1500ppm, antimony 500-1500ppm, strontium 800-1500ppm, calcium 500-1000ppm, sulfate 800-1500ppm, the rest is active MgO.

Citation Information

Patent Citations

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