Supported solid alkali deacidification and dehydration material and preparation method thereof

Abstract

The invention provides a supported solid alkali deacidification and dehydration material and a preparation method thereof.The preparation method of the supported solid alkali deacidification and dehydration material comprises the steps that 1, gamma-aluminum oxide, magnesium hydroxide and starch are mixed and kneaded for the first time, and a dry mixture is obtained; (2) adding an acid solvent and an alcohol solvent into the dry mixture, and carrying out secondary mixing and kneading to obtain a wet mixture; (3) extruding, granulating, drying and calcining the wet mixture to obtain a first precursor; (4) grinding and mixing calcium carbide and the first precursor to obtain a second precursor; and (5) packaging the second precursor by adopting PP melt-blown cloth to obtain the supported solid alkali deacidification and dehydration material. When the supported solid alkali deacidification and dehydration material is used, solid impurities can be effectively prevented from being attached to the surface to influence the activity of the material, and the loss of the material can be effectively avoided, so that the deacidification and dehydration efficiency is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of the preparation of deacidification and dehydration materials, and particularly relates to a supported solid base deacidification and dehydration material and a preparation method thereof. Background Art

[0002] The main components of the electrolyte include electrolyte salts, organic solvents, and additives. Taking lithium-ion batteries as an example, the electrolyte salt usually uses lithium hexafluorophosphate. Lithium hexafluorophosphate has a certain moisture sensitivity and will react with water to generate acidic substances such as hydrogen fluoride, so that the lithium hexafluorophosphate raw material will contain a certain amount of hydrogen fluoride. The organic solvents include carbonate solvents, carboxylate solvents, and ether solvents, etc. There may also be some moisture and hydroxyl-containing compounds in these solvents. Therefore, in addition to directly introducing hydrofluoric acid, the raw materials used in the production process of the electrolyte will also introduce moisture and hydroxyl-containing compounds. These moisture and hydroxyl-containing compounds react with lithium hexafluorophosphate to further generate acidic substances such as hydrogen fluoride. These acidic substances will corrode the electrode sheets during the battery cycle, resulting in a reduction in battery life and even triggering safety accidents. Therefore, the moisture and acid value of the electrolyte must be strictly controlled. However, in the actual production process, only management means such as improving the raw material standards, molecular sieve dehydration, and temperature control can be adopted for control. Once products with unqualified acid values appear, they can only be treated as waste, which is neither environmentally friendly nor economical.

[0003] At present, there are also some existing technologies that use MgO as an adsorbent for deacidification and dehydration. As a solid base, MgO is widely used because of its advantages such as high deacidification efficiency, low cost, easy availability, stable deacidification products, insoluble in organic solvents, and strong anti-loss ability. However, in the process of deacidification and dehydration of the existing MgO solid base adsorbent, as the acid and water continuously react with MgO, the generated Mg(OH) 2 or salts and other impurities adhere to its surface, thereby blocking the deacidification and dehydration process and reducing the deacidification and dehydration efficiency. Therefore, it is urgent to develop a new solid base deacidification and dehydration material to solve the deficiencies of the existing technologies. Summary of the Invention

[0004] The purpose of the present invention is to provide a supported solid base deacidification and dehydration material and a preparation method thereof. When the supported solid base deacidification and dehydration material is used, it can effectively avoid the attachment of product impurities to the surface and affect its activity, and can effectively avoid the loss of the material, thereby improving the deacidification and dehydration efficiency.

[0005] To achieve the above purpose, on the one hand, the present invention provides a preparation method of a supported solid base deacidification and dehydration material, including the steps of: (1) Kneading γ-aluminum oxide, magnesium hydroxide, and starch for the first time to obtain a dry blend; (2) Add an acid solvent and an alcohol solvent to the dry mixture and perform secondary kneading to obtain a wet mixture; (3) Extrude, granulate, dry, and calcine the wet mixture to obtain a first precursor; (4) Grind and mix calcium carbide and the first precursor to obtain a second precursor, and the mass ratio of calcium carbide to the first precursor is 0.5 - 50:100; (5) Package the second precursor with a PP meltblown fabric to obtain a supported solid base deacidification and dehydration material.

[0006] Compared with the prior art, the present invention has at least the following beneficial effects: (1) In the present invention, magnesium hydroxide is loaded on γ-aluminum oxide by a kneading method with starch as a binder, which improves the bonding strength between materials. Then, through calcination, a first precursor containing magnesium oxide solid base is generated, and calcium carbide is introduced into the first precursor to obtain a second precursor. Calcium carbide can react with acid and water to produce gas, which can disturb the interface, effectively avoiding the attachment of impurities such as magnesium hydroxide or salts on the surface, maintaining the interface activity, and thus effectively improving the deacidification and dehydration efficiency of the supported solid base deacidification and dehydration material of the present invention.

[0007] (2) The present invention uses an acid solvent and an alcohol solvent to perform secondary kneading on the dry mixture, which helps to further mix the raw materials, is convenient for subsequent extrusion granulation and forming, and at the same time, the acid solvent and alcohol solvent contained decompose or volatilize to release gas during the calcination process, thereby achieving a pore-forming effect, improving the specific surface area of the material, and further effectively increasing the contact area between the material and acid and water, which helps to improve its deacidification and dehydration efficiency.

[0008] (3) The present invention uses a PP meltblown fabric to package the second precursor. The PP meltblown fabric has many pores, a fluffy structure, can achieve a good filtering effect, and can effectively avoid the loss of the material, thereby ensuring its deacidification and dehydration efficiency.

[0009] In summary, the supported solid base deacidification and dehydration material prepared by the preparation method of the present invention can effectively avoid the loading of generated impurities on its surface, and can effectively avoid the loss of the material, improving the deacidification and dehydration efficiency.

[0010] Further, the mass ratio of the γ-aluminum oxide, the magnesium hydroxide, and the starch is 1000:100 - 300:1.

[0011] Further, both the first kneading and the second kneading are carried out in a kneader.

[0012] Further, the time of the first kneading is 5 min - 240 min, and the rotation speed is 0 rpm - 120 rpm.

[0013] Furthermore, the time for the secondary kneading is 5 min to 120 min, and the rotation speed is 5 rpm to 100 rpm.

[0014] Furthermore, the acid solvent is selected from at least one of nitric acid and acetic acid.

[0015] Furthermore, the alcohol solvent is selected from at least one of ethylene glycol and glycerol.

[0016] Furthermore, the mass ratio of the dry blend, the acid solvent, and the alcohol solvent is 1000:50 to 300:1 to 100.

[0017] Furthermore, the extrusion granulation is carried out in a screw extruder, and the diameter of the material obtained after the extrusion granulation is 3 mm to 5 mm, and the length is 0.5 cm to 10 cm.

[0018] Furthermore, the temperature of the drying is 50 °C to 110 °C, and the time of the drying is 6 h to 24 h.

[0019] Furthermore, the temperature of the calcination is 400 °C to 580 °C, and the time of the calcination is 1 h to 4 h.

[0020] Furthermore, the particle size Dv50 of the second precursor is 0.01 mm to 3 mm.

[0021] On the other hand, the present invention provides a supported solid base deacidification and dehydration material, which is prepared by using the preparation method of the supported solid base deacidification and dehydration material described above. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is the supported solid base deacidification and dehydration material prepared in Example 1 of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0023] The preparation method of the supported solid base deacidification and dehydration material of the present invention includes the steps of: (1) Kneading γ-aluminum oxide, magnesium hydroxide, and starch for the first time to obtain a dry blend; (2) Adding an acid solvent and an alcohol solvent to the dry blend and kneading for the second time to obtain a wet blend; (3) Extruding, granulating, drying, and calcining the wet blend to obtain a first precursor; (4) Grinding and mixing calcium carbide and the first precursor to obtain a second precursor; (5) Packaging the second precursor with a PP melt-blown cloth to obtain a supported solid base deacidification and dehydration material.

[0024] In step (1), the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch is 1000:100 - 300:1. In some technical solutions, the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch is 1000:100:1. In some technical solutions, the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch is 1000:136:1. In some technical solutions, the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch is 1000:300:1. As an example, the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch can be, but is not limited to, 1000:100:1, 1000:120:1, 1000:140:1, 1000:160:1, 1000:180:1, 1000:200:1, 1000:220:1, 1000:240:1, 1000:260:1, 1000:280:1, 1000:300:1. The first kneading is carried out in a kneader, and the time of the first kneading is 5 min - 240 min. As an example, the time of the first kneading can be, but is not limited to, 5 min, 10 min, 20 min, 30 min, 50 min, 80 min, 100 min, 120 min, 140 min, 160 min, 180 min, 200 min, 220 min, 240 min, and the rotation speed is 0 rpm - 120 rpm. As an example, the rotation speed of the first kneading can be, but is not limited to, 0 rpm, 10 rpm, 20 rpm, 40 rpm, 60 rpm, 80 rpm, 100 rpm, 120 rpm. Magnesium hydroxide is the raw material for preparing magnesium oxide solid base. Preferably, the magnesium hydroxide of the present invention is high-purity magnesium hydroxide; γ-aluminum oxide is an inorganic compound with high thermal stability and excellent mechanical properties, which has a high specific surface area and good pore structure. In the present invention, magnesium hydroxide is loaded on the γ-aluminum oxide matrix by the kneading method, and starch is used as a binder to improve the strength of the overall material structure.

[0025] In step (2), the acid solvent is selected from at least one of nitric acid and acetic acid. Preferably, the acid solvent is selected from nitric acid, and more preferably, the acid solvent is nitric acid with a mass percentage of 20% - 30%. The alcohol solvent is selected from at least one of ethylene glycol and glycerol. Preferably, the alcohol solvent is selected from ethylene glycol. The mass ratio of the dry blend, acid solvent, and alcohol solvent is 1000:50 - 300:1 - 100. In some technical solutions, the mass ratio of the dry blend, acid solvent, and alcohol solvent is 1000:80 - 260:10 - 80. As an example, the mass ratio of the dry blend, acid solvent, and alcohol solvent can be, but is not limited to, 1000:50:10, 1000:50:20, 1000:50:40, 1000:50:60, 1000:50:80, 1000:50:100, 1000:80:10, 1000:80:20, 1000:80:40, 1000:80:60, 1000:80:80, 1000:80:100, 1000:100:10, 1000:100:20, 1000:100:40, 1000:100:60, 1000:100:80, 1000:100:100, 1000:200:10, 1000:200:20, 1000:200:40, 1000:200:60, 1000:200:80, 1000:200:100, 1000:300:10, 1000:300:20, 1000:300:40, 1000:300:60, 1000:300:80, 1000:300:100. The addition of the acid solvent and alcohol solvent can further mix the raw materials for subsequent extrusion granulation and forming; at the same time, the acid solvent can react with magnesium hydroxide to obtain magnesium salt, and the magnesium salt will decompose during calcination to obtain magnesium oxide with higher activity; and the alcohol solvent and the unreacted acid solvent will decompose or volatilize during calcination, thus achieving the effect of pore formation on the material, increasing the specific surface area of the material, and further effectively increasing the contact area between the solid base material and acid and water, improving the acid and water removal effect. The secondary kneading can be carried out in a kneader, and the time for secondary kneading is 5 min - 120 min. As an example, the time for secondary kneading can be, but is not limited to, 5 min, 10 min, 20 min, 30 min, 50 min, 80 min, 100 min, 120 min. The rotation speed for secondary kneading is 5 rpm - 100 rpm. As an example, the rotation speed for secondary kneading can be, but is not limited to, 5 rpm, 10 rpm, 20 rpm, 30 rpm, 40 rpm, 50 rpm, 60 rpm, 70 rpm, 80 rpm, 90 rpm, 100 rpm.

[0026] In step (3), extrusion granulation is carried out in a screw extruder. The wet mixture enters the screw extruder for extrusion to obtain a strip with a diameter of 3 mm to 5 mm, and the strip is cut into materials with a length of 0.5 to 10 cm. Then the materials are dried. The drying can be carried out in an oven, and the drying temperature is 50°C to 110°C. As an example, the drying temperature can be but is not limited to 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, 110°C. The drying time is 6 h to 24 h. As an example, the drying time can be but is not limited to 6 h, 7 h, 8 h, 9 h, 10 h, 12 h, 14 h, 16 h, 18 h, 20 h, 22 h, 24 h. Calcination can be carried out in a muffle furnace, and the calcination temperature is 400°C to 580°C. As an example, the calcination temperature can be but is not limited to 400°C, 410°C, 420°C, 430°C, 440°C, 450°C, 460°C, 470°C, 480°C, 490°C, 500°C, 510°C, 520°C, 530°C, 540°C, 550°C, 560°C, 570°C, 580°C. The calcination time is 1 h to 4 h. As an example, the calcination time can be but is not limited to 1 h, 2 h, 3 h, 4 h. During the process of heating up for calcination, the acidic solvent contained in the wet mixture can react with magnesium hydroxide to generate magnesium salts. At the same time, as the temperature rises, the alcohol solvent and the unreacted acidic solvent are decomposed or volatilized, thus forming pores on the material surface to increase the specific surface area of the material and further improve its adsorption treatment effect. And magnesium hydroxide and magnesium salts are further decomposed at the calcination temperature to obtain solid base magnesium oxide.

[0027] In step (4), the mass ratio of calcium carbide to the first precursor is 0.5 - 50:100. In some technical solutions, the mass ratio of calcium carbide to the first precursor is 0.5 - 30:100. In some technical solutions, the mass ratio of calcium carbide to the first precursor is 1 - 10:100. As an example, the mass ratio of calcium carbide to the first precursor can be, but is not limited to, 0.5:100, 1:100, 2:100, 4:100, 6:100, 8:100, 10:100, 20:100, 30:100, 40:100, 50:100. The grinding and mixing can be carried out in a ball mill with a nitrogen atmosphere. The particle size Dv50 of the obtained second precursor after grinding and mixing can be 0.01 mm - 3 mm. As an example, the particle size Dv50 of the second precursor can be, but is not limited to, 0.01 mm, 0.05 mm, 0.1 mm, 0.2 mm, 0.4 mm, 0.5 mm, 0.6 mm, 0.8 mm, 1 mm, 1.2 mm, 1.4 mm, 1.6 mm, 1.8 mm, 2 mm, 2.2 mm, 2.4 mm, 2.6 mm, 2.8 mm, 3 mm. Calcium carbide can react with acid and water to produce gas, which can disturb the interface, effectively avoid the attachment of magnesium hydroxide or salt impurities generated during the adsorption treatment of solid base to acid or water on its surface, maintain the interface activity, and achieve a better dehydration and deacidification effect. And grinding and mixing calcium carbide and the first precursor can further increase the specific surface area of the material and thus improve its activity, which helps to further improve the deacidification and dehydration efficiency of the material.

[0028] In step (5), the PP meltblown fabric has many voids, a fluffy structure, good anti-wrinkle ability, and good performance such as filtration and shielding. Using the PP meltblown fabric to package the second precursor can achieve a good filtration effect and effectively avoid the loss of materials. The volume of the PP meltblown fabric can be 50 mL, 60 mL, 70 mL, 80 mL, 90 mL, 100 mL, 200 mL, but is not limited thereto.

[0029] The present invention also provides a supported solid base deacidification and dehydration material prepared by the preparation method of the supported solid base deacidification and dehydration material described above.

[0030] To better illustrate the purpose, technical solution and beneficial effects of the present invention, the present invention will be further described below in conjunction with specific embodiments. It should be noted that the methods described in the following embodiments are further explanatory descriptions of the present invention and should not be regarded as limitations of the present invention.

[0031] Example 1 This example is a preparation method of a supported solid base deacidification and dehydration material, including the steps: (1) γ-aluminum oxide, magnesium hydroxide, and starch are subjected to primary kneading to obtain a dry blend. Among them, the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch is 1000:136:1. The primary kneading is carried out in a kneader. The time for primary kneading is 5 min, and the rotation speed is 50 rpm. (2) An acid solvent and an alcohol solvent are added to the dry blend for secondary kneading to obtain a wet blend. Among them, the mass ratio of the dry blend, the acid solvent, and the alcohol solvent is 1000:100:10. The acid solvent is selected from nitric acid (mass percentage is 25%), and the alcohol solvent is selected from ethylene glycol. The secondary kneading is carried out in a kneader. The time for secondary kneading is 60 min, and the rotation speed is 50 rpm. (3) The wet blend is extruded through a screw extruder to obtain a strip with a diameter of 4 mm, and the strip is cut into materials with a length of 10 cm. The materials are dried at 110 °C for 24 h and then calcined at 580 °C for 4 h to obtain a first precursor. (4) Calcium carbide and the first precursor are ground and mixed according to a mass ratio of 5:100 to obtain a second precursor with a Dv50 particle size of 1 mm. (5) The second precursor is packaged with 50 mL of PP melt-blown fabric to obtain a supported solid base deacidification and dehydration material with a volume of 50 mL, as Figure 1 shown.

[0032] Example 2 This example is a preparation method of a supported solid base deacidification and dehydration material, including the steps: (1) γ-aluminum oxide, magnesium hydroxide, and starch are subjected to primary kneading to obtain a dry blend. Among them, the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch is 1000:300:1. The primary kneading is carried out in a kneader. The time for primary kneading is 5 min, and the rotation speed is 50 rpm. (2) An acid solvent and an alcohol solvent are added to the dry blend for secondary kneading to obtain a wet blend. Among them, the mass ratio of the dry blend, the acid solvent, and the alcohol solvent is 1000:100:10. The acid solvent is selected from nitric acid (mass percentage is 25%), and the alcohol solvent is selected from ethylene glycol. The secondary kneading is carried out in a kneader. The time for secondary kneading is 60 min, and the rotation speed is 50 rpm. (3) The wet blend is extruded through a screw extruder to obtain a strip with a diameter of 5 mm, and the strip is cut into materials with a length of 10 cm. The materials are dried at 110 °C for 24 h and then calcined at 580 °C for 4 h to obtain a first precursor. (4) Calcium carbide and the first precursor are ground and mixed according to a mass ratio of 5:100 to obtain a second precursor with a Dv50 particle size of 1 mm. (5) The second precursor is packaged with 50 mL of PP melt-blown fabric to obtain a supported solid base deacidification and dehydration material with a volume of 50 mL.

[0033] Example 3 This example is a preparation method of a supported solid base deacidification and dehydration material, including the steps: (1) γ-aluminum oxide, magnesium hydroxide, and starch are subjected to primary kneading to obtain a dry mixture. Among them, the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch is 1000:220:1. The primary kneading is carried out in a kneader. The time of primary kneading is 10 min, and the rotation speed is 100 rpm; (2) An acid solvent and an alcohol solvent are added to the dry mixture for secondary kneading to obtain a wet mixture. Among them, the mass ratio of the dry mixture, the acid solvent, and the alcohol solvent is 1000:300:100. The acid solvent is selected from acetic acid, and the alcohol solvent is selected from glycerol. The secondary kneading is carried out in a kneader. The time of secondary kneading is 30 min, and the rotation speed is 80 rpm; (3) The wet mixture is extruded through a screw extruder to obtain a strip with a diameter of 5 mm. The strip is cut into materials with a length of 5 cm. The materials are dried at 70 °C for 24 h and then calcined at 500 °C for 4 h to obtain a first precursor; (4) Calcium carbide and the first precursor are ground and mixed according to a mass ratio of 10:100 to obtain a second precursor with a Dv50 particle size of 3 mm; (5) The second precursor is packaged with 50 mL of PP melt-blown cloth to obtain a supported solid base deacidification and dehydration material with a volume of 50 mL.

[0034] Comparative Example 1 This comparative example is a preparation method of a supported solid base deacidification and dehydration material, including the steps: (1) γ-aluminum oxide, magnesium hydroxide, and starch are subjected to primary kneading to obtain a dry mixture. Among them, the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch is 1000:136:1. The primary kneading is carried out in a kneader. The time of primary kneading is 5 min, and the rotation speed is 50 rpm; (2) An acid solvent and an alcohol solvent are added to the dry mixture for secondary kneading to obtain a wet mixture. Among them, the mass ratio of the dry mixture, the acid solvent, and the alcohol solvent is 1000:100:10. The acid solvent is selected from nitric acid (mass percentage 25%), and the alcohol solvent is selected from ethylene glycol. The secondary kneading is carried out in a kneader. The time of secondary kneading is 60 min, and the rotation speed is 50 rpm; (3) The wet mixture is extruded through a screw extruder to obtain a strip with a diameter of 4 mm, and the strip is cut into materials with a length of 10 cm. The materials are dried at 110 °C for 24 h and then calcined at 580 °C for 4 h to obtain a first precursor; (4) The first precursor is ground to obtain a second precursor with a Dv50 particle size of 1 mm; (5) The second precursor was packaged with 50 mL of PP meltblown fabric to obtain a supported solid base deacidification and dehydration material with a volume of 50 mL.

[0035] Comparative Example 2 This comparative example is a preparation method of a supported solid base deacidification and dehydration material, including the steps: (1) γ-alumina, magnesium hydroxide, and starch were subjected to primary kneading to obtain a dry mixture. Among them, the mass ratio of γ-alumina, magnesium hydroxide, and starch was 1000:136:1. The primary kneading was carried out in a kneader. The time of primary kneading was 5 min, and the rotation speed was 50 rpm; (2) An acid solvent and an alcohol solvent were added to the dry mixture for secondary kneading to obtain a wet mixture. Among them, the mass ratio of the dry mixture, the acid solvent, and the alcohol solvent was 1000:100:10. The acid solvent was selected from nitric acid (mass percentage 25%), and the alcohol solvent was selected from ethylene glycol. The secondary kneading was carried out in a kneader. The time of secondary kneading was 60 min, and the rotation speed was 50 rpm; (3) The wet mixture was extruded through a screw extruder to obtain a strip with a diameter of 4 mm. The strip was cut into materials with a length of 10 cm. The materials were dried at 110 °C for 24 h and then calcined at 580 °C for 4 h to obtain a first precursor; (4) Calcium carbide and the first precursor were ground and mixed at a mass ratio of 0.3:100 to obtain a second precursor with a Dv50 particle size of 1 mm; (5) The second precursor was packaged with 50 mL of PP meltblown fabric to obtain a supported solid base deacidification and dehydration material with a volume of 50 mL.

[0036] Comparative Example 3 This comparative example is a preparation method of a supported solid base deacidification and dehydration material, including the steps: (1) γ-alumina, magnesium hydroxide, and starch were subjected to primary kneading to obtain a dry mixture. Among them, the mass ratio of γ-alumina, magnesium hydroxide, and starch was 1000:136:1. The primary kneading was carried out in a kneader. The time of primary kneading was 5 min, and the rotation speed was 50 rpm; (2) An alcohol solvent was added to the dry mixture for secondary kneading to obtain a wet mixture. Among them, the mass ratio of the dry mixture, water, and the alcohol solvent was 1000:100:10. The alcohol solvent was selected from ethylene glycol. The secondary kneading was carried out in a kneader. The time of secondary kneading was 60 min, and the rotation speed was 50 rpm; (3) The wet mixture was extruded through a screw extruder to obtain a strip with a diameter of 4 mm, and the strip was cut into materials with a length of 10 cm. The materials were dried at 110 °C for 24 h and then calcined at 580 °C for 4 h to obtain a first precursor; (4)Mix calcium carbide and the first precursor in a mass ratio of 5:100 by grinding to obtain a second precursor with a Dv50 particle size of 1 mm. (5)Pack the second precursor with a 50 mL PP meltblown cloth to obtain a supported solid base deacidification and dehydration material with a volume of 50 mL.

[0037] Comparative Example 4 This comparative example is a preparation method of a supported solid base deacidification and dehydration material, including the steps: (1)Perform primary kneading on γ-aluminum oxide, magnesium hydroxide, and starch to obtain a dry mixture. Among them, the mass ratio of γ-aluminum oxide, magnesium hydroxide, and starch is 1000:136:1. The primary kneading is carried out in a kneader. The time of the primary kneading is 5 min, and the rotation speed is 50 rpm. (2)Add an alcohol solvent to the dry mixture for secondary kneading to obtain a wet mixture. Among them, the mass ratio of the dry mixture to the alcohol solvent is 1000:100:10. The alcohol solvent is selected from ethylene glycol. The secondary kneading is carried out in a kneader. The time of the secondary kneading is 60 min, and the rotation speed is 50 rpm. (3)Extrude the wet mixture through a screw extruder to obtain a strip with a diameter of 4 mm. Cut the strip into materials with a length of 10 cm. Dry the materials at 110 °C for 24 h, and then calcine them at 580 °C for 4 h to obtain the first precursor. (4)Mix calcium carbide and the first precursor in a mass ratio of 5:100 by grinding to obtain a second precursor with a Dv50 particle size of 1 mm, which is also the supported solid base deacidification and dehydration material.

[0038] Place the supported solid base deacidification and dehydration materials with a volume of 50 mL (dry weight of 41.00 g) prepared in Examples 1 to 3 and Comparative Examples 1 to 4 into a stainless steel fixed bed with an inner diameter of 20 cm, introduce the electrolyte, and control the flow rate of the electrolyte to be 5 m 3 / h (the acid value of the electrolyte is 140 ppm, the moisture content is 35 ppm, and the total volume is 20 L). Finally, analyze the acid value and moisture content of the deacidified and dehydrated electrolyte, and weigh the supported solid base deacidification and dehydration materials of each example and comparative example after drying in a vacuum drying oven at 35 °C for 24 h. The analysis and test results are shown in Table 1.

[0039] Table 1 Analysis and test results of Examples 1 to 3 and Comparative Examples 1 to 4

[0040] Specifically, please refer to the analysis results in Table 1. It can be seen from the analysis results of Examples 1 to 3 and Comparative Examples 1 to 4 that the supported solid base deacidification and dehydration material prepared by the preparation method of the present invention has better deacidification and dehydration effects.

[0041] Further comparing the results of Example 1 and Comparative Examples 1-2, it can be seen that when calcium carbide is missing or the addition amount of calcium carbide is less than the scope of the present invention, the effects of deacidification and dehydration will be affected, indicating that adding a certain amount of calcium carbide is beneficial to improving the deacidification and dehydration performance of the supported solid base deacidification and dehydration material of the present invention. From the analysis results of Example 1 and Comparative Examples 3-4, it can be seen that when the acid solvent is replaced with water, it has a significant impact on the deacidification and dehydration effects of the solid base; when the second precursor is not packaged, the loss of the solid base deacidification and dehydration material is serious, and thus the deacidification and dehydration effects are reduced to a certain extent.

[0042] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, it is not limited to only the embodiments listed. Those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for preparing a supported solid base deacidification and dehydration material, characterized in that: Includes steps: (1) kneading γ-alumina, magnesium hydroxide and starch to obtain a dry mix; (2) adding an acid solvent and an alcohol solvent to the dry mixture and kneading the mixture for a second time to obtain a wet mixture; (3) extruding, granulating, drying, and calcining the wet mixture to obtain a first precursor; (4) grinding and mixing calcium carbide and the first precursor to obtain a second precursor, wherein the mass ratio of the calcium carbide to the first precursor is 0.5-50:100; (5) The second precursor is packaged with PP melt-blown cloth to obtain a supported solid alkali deacidification and dehydration material.

2. The method for preparing a supported solid base deacidification and dehydration material according to claim 1, characterized in that: The mass ratio of the γ-alumina, the magnesium hydroxide and the starch is 1000:100-300:

1.

3. The method for preparing a supported solid base deacidification and dehydration material according to claim 1, characterized in that: The first kneading and the second kneading are both carried out in a kneading machine, the first kneading time is 5min~240min, the rotation speed is 0rpm~120rpm, the second kneading time is 5min~120min, and the rotation speed is 5rpm~100rpm.

4. The method for preparing a supported solid base deacidification and dehydration material according to claim 1, characterized in that: The acid solvent is selected from at least one of nitric acid and acetic acid, and the alcohol solvent is selected from at least one of ethylene glycol and glycerol.

5. The method for preparing a supported solid base deacidification and dehydration material according to claim 1, characterized in that: The mass ratio of the dry blend, the acid solvent and the alcohol solvent is 1000:50-300:1-100.

6. The method for preparing a supported solid base deacidification and dehydration material according to claim 1, characterized in that: The extrusion granulation is carried out in a screw extruder, and the diameter of the material obtained after the extrusion granulation is 3mm~5mm, and the length is 0.5cm~10cm.

7. The method for preparing a supported solid base deacidification and dehydration material according to claim 1, characterized in that: The drying temperature is 50° C. to 110° C., and the drying time is 6 h to 24 h.

8. The method for preparing a supported solid base deacidification and dehydration material according to claim 1, characterized in that: The calcination temperature is 400° C. to 580° C., and the calcination time is 1 h to 4 h.

9. The method for preparing a supported solid base deacidification and dehydration material according to claim 1, characterized in that: The particle size Dv50 of the second precursor is 0.01 mm to 3 mm.

10. A supported solid alkali deacidification and dehydration material, characterized in that: The deacidification and dehydration material is prepared by the preparation method of the supported solid alkali deacidification and dehydration material according to any one of claims 1 to 9.

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