Method for preparing sodium ion water by normal-temperature solid-phase circulation reaction and closed-loop circulation system

Abstract

The application discloses a method for preparing sodium ion water through normal-temperature solid-phase circulation reaction and a closed-loop circulation system, and belongs to the technical field of sodium ion water solution preparation. The method uses metal calcium powder and sodium fluoride powder as main raw materials, mixes them in proportion, slightly humidifies, and then high-pressure presses into a square block, and then performs aging reaction under normal-temperature ventilation conditions; after aging is completed, the square block is crushed and broken, and then is put into water for leaching to obtain a sodium ion-containing water solution; fluorine ion detection is performed on the leaching solution, if fluorine is contained, calcium fluoride precipitate is generated by in-situ reaction through adding metal calcium powder, and then pure sodium ion water is obtained after filtration; the wet filter residue generated in the filtration is not subjected to drying treatment, and new sodium fluoride dry powder and metal calcium dry powder are directly supplemented in proportion, and then are mixed, pressed into a block, aged, and leached again, so that the raw materials are used in a closed-loop circulation mode for unlimited times. The application is safe and stable in the whole process under normal temperature and normal pressure, does not generate waste materials and does not emit pollutants, can continuously prepare sodium ion water in a low cost and large batch, solves the problems of low conversion rate, raw material waste and complex process in traditional solid-solid reaction, and is suitable for large-scale, environmentally-friendly and safe production of sodium ion water solution.

Description

Technical Field

[0001] This invention belongs to the field of sodium ion aqueous solution preparation technology, specifically relating to a method for preparing high-purity sodium ion water by solid-phase circulating reaction at room temperature and its fluoride salt closed-loop circulation system, which is particularly suitable for low-cost, continuous and environmentally friendly production of food-grade, chlorine-free, and low-impurity sodium ion water. Background Technology

[0002] Currently, the preparation of sodium ion water mainly employs electrolysis, ion exchange, and mineral leaching methods, which generally suffer from problems such as high equipment investment, high energy consumption, harsh reaction conditions, low conversion rates, and difficult-to-treat byproducts. While traditional solid-solid displacement reactions can generate sodium ions, the calcium fluoride produced during the reaction forms a dense coating, preventing further reaction of the internal raw materials, resulting in low raw material utilization and incomplete reaction. Furthermore, existing technologies generally suffer from drawbacks such as the need to dry filter residue, cumbersome processes, high material losses, and the inability to achieve closed-loop recycling, making it difficult to achieve low-cost, continuous, and environmentally friendly production. Therefore, the market urgently needs a new process method specifically designed for the preparation of sodium ion water that is safe, operates at room temperature and pressure, is recyclable, and produces zero waste. Summary of the Invention

[0003] Purpose of the invention: To provide a method for continuously preparing sodium ion water through solid-phase circulating reaction at room temperature and pressure, achieving 100% utilization of raw materials, no waste discharge, mild and controllable reaction, simple process, and unlimited recycling.

[0004] Technical Solution: 1. Ingredient Mixing: Calcium metal powder and sodium fluoride powder are mixed evenly according to a specific mass ratio. 2. Humidification and Briquetting: A small amount of water is added for humidification, and the mixture is pressed into dense cubes using hydraulic equipment under high pressure to increase the contact area and promote a slow reaction. 3. Aging at Room Temperature: The mixture is piled up and aged in a well-ventilated environment free of flammable materials at room temperature, allowing a mild displacement reaction between calcium and sodium fluoride to produce sodium metal and calcium fluoride. 4. Crushing and Shell Breaking: After aging, the mixture is crushed to break the calcium fluoride coating and expose the unreacted raw materials inside. 5. Sodium Extraction through Sodium Sodium Extraction: The crushed material is added to water, where sodium metal reacts with water to produce an aqueous solution of sodium ions. 6. Defluorination and Purification: Fluoride ion levels in the water are tested. If the levels are too high, calcium powder is added to react and produce calcium fluoride precipitate. 7. Product Filtration: Pure sodium ion water is obtained after filtration. 8. Direct Recycling of Wet Residue: The filter residue is kept moist, without drying, and is directly replenished with new sodium fluoride powder and calcium powder, then briquetted again for recycling.

[0005] Advantages of this invention: Operating at room temperature and pressure, safe with no high temperature or explosion risk; The block shape is easy to stack, store, and transport; Crushing and shell breaking solves the problem of low conversion rate; Wet residue is directly recycled, eliminating the drying step, resulting in energy saving and high efficiency; Calcium powder undergoes in-situ defluorination, leaving no fluoride residue or waste; The entire process is closed-loop, with zero emissions and zero waste; It can be recycled indefinitely, continuously producing sodium ion water. Detailed implementation method: Example 1: 1. Take 100 parts of metallic calcium powder and 210 parts of sodium fluoride powder, and mix them evenly. 2. Add 1.5% to 2% of the total mass of purified water and stir until slightly moist. 3. Press the mixture into 5cm×5cm×5cm cubes using a hydraulic press at a pressure of 20-35MPa. 4. Aging the cubes for 3-7 days in a well-ventilated room at 20℃ with no combustibles. 5. After aging, pulverize the cubes into granules. 6. Immerse the cubes in clean water for 30 minutes to obtain an aqueous solution containing sodium ions. 7. Detect fluoride ions; if present, add calcium powder and stir until the fluoride ions are completely precipitated. 8. Filter to obtain a sodium ion aquatic product. 9. Do not dry the filter residue; directly add calcium powder and sodium fluoride powder to the original ratio, mix, and press into cubes again for recycling. Example 2: 1. Prepare the mixture according to a calcium:sodium fluoride mass ratio of 1:2.1. 2. Add a small amount of moisture and press into cubes under high pressure. 3. Aging at room temperature for 3-15 days. 4. Crushing, soaking in water, defluorination, and filtering. 5. The wet filter residue is directly used to replenish fresh material for cyclical production. Attached image description: Figure 1 : Process flow diagram of the present invention 1. Ingredient preparation → 2. Humidification and pressing → 3. Aging at room temperature → 4. Crushing and shell breaking → 5. Soaking in water to extract sodium → 6. Defluoridation with calcium powder → 7. Filtration → 8. Finished sodium ion water 2. Filter residue → Add new material → Return to step 2.

Claims

1. A method for preparing sodium-ion water via a solid-phase cyclic reaction at room temperature, characterized in that, Includes the following steps: (1) Mix the calcium metal powder and sodium fluoride powder evenly according to the mass ratio; (2) Add a trace amount of water to humidify, and press under high pressure to form a dense cube; (3) Place the cube in a room temperature, ventilated environment free of flammable materials for aging reaction; (4) After aging, crush the calcium fluoride coating to destroy it; (5) The crushed material is put into water for extraction to obtain an aqueous solution containing sodium ions; (6) Detect fluoride ions in the extract. If it contains fluoride, add metallic calcium powder to react and generate calcium fluoride precipitate. (7) Pure sodium ion water is obtained by filtration. The wet filter residue produced by filtration is not dried. Sodium fluoride powder and metallic calcium powder are added directly, and the mixture is mixed, pressed, aged and extracted again to achieve a closed loop cycle.

2. The method according to claim 1, characterized in that, The mass ratio of metallic calcium powder to sodium fluoride powder is 1:2.

1.

3. The method according to claim 1, characterized in that, The amount of humidifying water is 1.5% to 2% of the total material mass.

4. The method according to claim 1, characterized in that, The pressing pressure is 20-35 MPa.

5. The method according to claim 1, characterized in that, The aging temperature is 15℃~30℃, and the aging time is 3 days~15 days.

6. The method according to claim 1, characterized in that, The wet filter residue is directly replenished with dry powder for circulation, without undergoing drying or desiccation steps.

7. The method according to claim 1, characterized in that, The defluorination process involves adding calcium powder in situ to generate calcium fluoride precipitate, which is then entirely recycled into the circulation system.

8. A closed-loop circulation system for preparing sodium ion water, characterized in that, It includes: a batching module, a briquetting module, an aging module, a crushing module, an extraction module, a defluorination module, a filtration module, and a circulating feed module; the wet filter residue produced by the filtration module directly enters the circulating feed module, and after replenishing with new raw materials, it re-enters the briquetting module, realizing a waste-free, unlimited closed-loop cycle throughout the entire process.

Images