A liquid additive for HiB silicon steel and a method of making the same
By employing atmospheric pressure reaction and adjusting trace elements in the production of HiB silicon steel, a liquid additive containing calcium was prepared, solving the problems of cumbersome high-pressure hydrothermal reaction and insufficient performance. This resulted in the low-cost and high-efficiency formation of magnesium silicate underlayer and the improvement of silicon steel performance.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- SHANGHAI SIIC ZHENTAI CHEM CO LTD
- Filing Date
- 2023-04-27
- Publication Date
- 2026-04-24
AI Technical Summary
The existing high-pressure hydrothermal reaction process in the production of HiB silicon steel is cumbersome and costly, and the existing liquid additives are not effective enough under normal pressure to form a dense magnesium silicate underlayer.
By replacing the high-pressure hydrothermal reaction with a reaction under normal pressure, adjusting the content of trace elements and increasing calcium, a liquid additive containing titanium, boron, antimony, strontium, calcium and sulfate is prepared. Clarity is ensured through stirring and dissolution processes, forming a highly efficient magnesium silicate underlayer.
It achieves safe and low-cost production, improves the fluidity and dispersibility of liquid additives, enhances the coatability of magnesium oxide slurry, improves the performance of silicon steel products, conforms to the concept of green chemistry, and has good product stability and long shelf life.
Abstract
Description
Technical Field
[0001] This invention relates to the field of metallurgy and chemical engineering, and in particular to a method for preparing a liquid additive suitable for HiB silicon steel. 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 in oriented silicon steel is used as a separating agent in the production of oriented silicon steel to prevent adhesion between steel coils at high temperatures. In addition, it reacts with silicon in the steel coil during high-temperature annealing to form a magnesium silicate underlayer. To ensure the underlayer grows in a specific grain direction, auxiliary additives containing a certain amount of trace elements are needed. The applicant previously developed a liquid additive and applied for Chinese patent CN202010877127.7, but the production process involves a high-pressure hydrothermal reaction, which is quite cumbersome. Summary of the Invention
[0003] The purpose of this invention is to provide a method for preparing liquid additives suitable for HiB silicon steel. Based on the above-mentioned patent, the production process has been upgraded by replacing the high-pressure hydrothermal reaction with a reaction under normal pressure. At the same time, the content of the original trace elements has been modified and calcium has been added to the original element types to improve the performance of the additive.
[0004] The technical solution adopted in this invention is as follows:
[0005] A liquid additive suitable for HiB silicon steel, comprising: titanium 500-1600ppm, boron 500-1600ppm, antimony 500-1500ppm, strontium 800-1200ppm, calcium 500-1000ppm, sulfate 800-1500ppm, with the remainder being H2O.
[0006] This invention adds calcium compared to Chinese patent CN202010877127.7. Because calcium is more metallic than magnesium and belongs to the same group, coating it onto the steel coil helps increase the reactivity of magnesium with silicon and iron in the coil, forming a more complete and dense magnesium silicate underlayer. 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 iron loss will decrease by about 0.1%. The preparation method of the above-mentioned liquid additive suitable for HiB silicon steel is as follows:
[0007] (1) Prepare a 40% to 80% mass fraction H2SO4 solution. Weigh out TiO2 according to the liquid additive suitable for HiB silicon steel with a Ti content of 500 to 1600 ppm. React and stir at 30 to 70°C for 15 to 40 minutes according to a solid-liquid mass ratio of 1:1 to 1:6 to obtain a pure clear solution.
[0008] (2) Weigh out SrCO3 according to the amount of Sr content in the liquid additive applicable to HiB silicon steel, which is 800 to 1200 ppm, and add it to the pure liquid obtained in step (1). Stir for 5 to 20 minutes to obtain a clear solution.
[0009] (3) Weigh out CaO in the amount of liquid additives suitable for HiB silicon steel with a Ca content of 500 to 1000 ppm and add it to the clear solution prepared in step (2). Stir for 5 to 20 minutes to obtain a clear solution.
[0010] (4) Weigh H3BO3 according to the amount of B content in the liquid additive applicable to HiB silicon steel, which is 500-1600ppm, and stir for 5-20 minutes at a material-to-water mass ratio of 1:1 to 1:4 to obtain a clear solution.
[0011] (5) Prepare a solvent with citric acid (C6H8O7) at a mass fraction of 5% to 50% and distilled water. Weigh out SbCl3 according to the amount of Sb content in the liquid additive suitable for HiB silicon steel at 500-1500ppm. Slowly add SbCl3 at a solid-liquid mass ratio of 1:1 to 1:4 while stirring until the solution is clear.
[0012] (6) Pour the solutions obtained in steps (3), (4) and (5) into a mixing tank and stir for 5-30 minutes to mix them.
[0013] Because titanium, antimony, and strontium readily hydrolyze in water to form insoluble precipitates or complexes, affecting their effectiveness, special attention must be paid to the clarity of the solution during preparation. This is also the focus of this solution.
[0014] The liquid additive of the present invention, suitable for HiB silicon steel, has the following advantages:
[0015] 1. This scheme uses dissolution and hydration reactions under normal pressure. Compared with the previously applied scheme, by adjusting the acid concentration and stirring conditions, dissolution under normal pressure can replace high-pressure dissolution. The method is simpler and safer, with lower production costs and is more low-carbon and environmentally friendly.
[0016] 2. The liquid additive obtained by this method has good fluidity and dispersibility, and can be better dispersed and fully mixed with magnesium oxide release agent during the stirring and preparation process, so that the additive effect can be best reflected.
[0017] 3. Compared with other additives, the addition of calcium can enhance the coating properties of magnesium oxide slurry and help improve the performance of silicon steel products.
[0018] 4. The product obtained by this method is clear and transparent, non-toxic, and has no special irritating odor;
[0019] 5. This method produces no intermediate by-products. Although there is a small amount of Sb heavy metal, the atom utilization rate is high and it will not cause Sb pollution. The reaction process is in line with the concept of green chemistry.
[0020] 6. The liquid obtained by this method is stable, has a long shelf life, is not prone to precipitation or deterioration, has simple storage conditions, and is convenient to transport. Detailed Implementation
[0021] The preferred embodiments of the present invention are given below to illustrate the technical solution of the present invention in detail.
[0022] Example 1
[0023] (1) Prepare a 40% mass fraction H2SO4 solution. Weigh out TiO2 according to the liquid additive suitable for HiB silicon steel with a Ti content of 500-1600ppm. React and stir at 30℃ for 40min at a solid-liquid mass ratio of 1:1 to obtain a pure solution.
[0024] (2) Weigh out SrCO3 according to the amount of liquid additive suitable for HiB silicon steel with Sr content of 800ppm and add it to the pure liquid obtained in step (1). Stir for 20 minutes to obtain a clear solution.
[0025] (3) Weigh out CaO according to the amount of liquid additives suitable for HiB silicon steel with a Ca content of 500ppm and add it to the clear solution prepared in step (2). Stir for 20 minutes to obtain a clear solution.
[0026] (4) Weigh out H3BO3 according to the amount of B content in the liquid additive applicable to HiB silicon steel at 500ppm, stir for 20min at a material-to-water mass ratio of 1:1 to obtain a clear solution.
[0027] (5) Prepare a solvent with citric acid (C6H8O7) at a mass fraction of 5% and distilled water. Weigh out SbCl3 according to the amount of Sb content in the liquid additive suitable for HiB silicon steel at 500ppm. Add SbCl3 at a solid-liquid mass ratio of 1:1 while stirring until the solution is clear.
[0028] (6) Pour the solutions obtained in steps (3), (4) and (5) into a mixing tank and stir for 30 minutes to mix them.
[0029] Example 2
[0030] (1) Prepare an 80% H2SO4 solution. Weigh out TiO2 according to the liquid additive suitable for HiB silicon steel with a Ti content of 1600ppm. React and stir at 70℃ for 15min according to a solid-liquid mass ratio of 1:6 to obtain a pure solution.
[0031] (2) Weigh out SrCO3 according to the amount of Sr content in the liquid additive applicable to HiB silicon steel with a content of 1200ppm and add it to the pure liquid obtained in step (1). Stir for 20 minutes to obtain a clear solution.
[0032] (3) Weigh out CaO according to the amount of liquid additives suitable for HiB silicon steel with a Ca content of 1000ppm and add it to the clear solution prepared in step (2). Stir for 20 minutes to obtain a clear solution.
[0033] (4) Weigh H3BO3 according to the amount of B content in the liquid additive applicable to HiB silicon steel at 1600ppm, stir for 5min at a material-to-water mass ratio of 1:4 to obtain a clear solution.
[0034] (5) Prepare a solvent with citric acid (C6H8O7) at a mass fraction of 50% and distilled water. Weigh out SbCl3 according to the amount of Sb content in the liquid additive suitable for HiB silicon steel at 1500ppm. Slowly add SbCl3 at a solid-liquid mass ratio of 1:4 while stirring until the solution becomes clear.
[0035] (6) Pour the solutions obtained in steps (3), (4) and (5) into a mixing tank and stir for 5 minutes to mix them evenly.
[0036] Example 3
[0037] (1) Prepare a 60% H2SO4 solution. Weigh out TiO2 according to the liquid additive suitable for HiB silicon steel with a Ti content of 1000ppm. React and stir at 50℃ for 30min according to a solid-liquid mass ratio of 1:4 to obtain a pure liquid.
[0038] (2) Weigh out SrCO3 according to the amount of Sr content in the liquid additive applicable to HiB silicon steel with a content of 1000ppm and add it to the pure liquid obtained in step (1). Stir for 10 minutes to obtain a clear solution.
[0039] (3) Weigh out CaO according to the amount of liquid additives suitable for HiB silicon steel with a Ca content of 800ppm and add it to the clear solution prepared in step (2). Stir for 10 minutes to obtain a clear solution.
[0040] (4) Weigh out H3BO3 according to the amount of B content in the liquid additive applicable to HiB silicon steel with a content of 1000ppm, stir for 10min at a material-to-water mass ratio of 1:2 to obtain a clear solution.
[0041] (5) Prepare a solvent with citric acid (C6H8O7) at a mass fraction of 30% and distilled water. Weigh out SbCl3 according to the amount of Sb content in the liquid additive suitable for HiB silicon steel at 1000ppm. Slowly add SbCl3 at a solid-liquid mass ratio of 1:2 while stirring until the solution becomes clear.
[0042] (6) Pour the solutions obtained in steps (3), (4) and (5) into a mixing tank and stir for 15 minutes to mix them.
[0043] 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 liquid additive suitable for HiB silicon steel, wherein the liquid additive, by mass fraction, comprises: titanium 500-1600 ppm, boron 500-1600 ppm, antimony 500-1500 ppm, strontium 800-1200 ppm, calcium 500-1000 ppm, sulfate 800-1500 ppm, with the remainder being H2O, characterized in that... Prepare according to the following steps: (1) Prepare a 40% to 80% mass fraction H2SO4 solution, weigh TiO2 according to the Ti content of 500 to 1600 ppm, react and stir at 30 to 70°C for 15 to 40 minutes according to the solid-liquid mass ratio of 1:1 to 1:6 to obtain a pure clear solution. (2) Weigh out SrCO3 with an Sr content of 800-1200 ppm and add it to the pure solution prepared in step (1). Stir for 5-20 minutes to obtain a clear solution. (3) Weigh out CaO with a Ca content of 500-1000 ppm and add it to the clear solution prepared in step (2). Stir for 5-20 minutes to obtain a clear solution. (4) Weigh out H3BO3 with a B content of 500-1600 ppm, stir for 5-20 min at a material-to-water mass ratio of 1:1 to 1:4, and obtain a clear solution. (5) Prepare a solvent with citric acid (C6H8O7) at a mass fraction of 5% to 50% and distilled water. Weigh out SbCl3 at a mass fraction of 500 to 1500 ppm and slowly add it to the solution at a solid-liquid mass ratio of 1:1 to 1:4 while stirring until the solution is clear. (6) Pour the solutions obtained in steps (3), (4) and (5) into a mixing tank and stir for 5 to 30 minutes to mix them.
Citation Information
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