Supported solid base deacidification and dehydration material and preparation method thereof

Abstract

The application provides a supported solid base deacidification and dewatering material and a preparation method thereof. The preparation method of the supported solid base deacidification and dewatering material comprises the following steps: (1) mixing γ-alumina, magnesium hydroxide and starch once to obtain dry mixture; (2) adding acid solvent and alcohol solvent to the dry mixture to perform secondary mixing to obtain wet mixture; (3) performing extrusion granulation, drying and calcination on the wet mixture to obtain first precursor; (4) grinding and mixing calcium carbide and the first precursor to obtain second precursor; and (5) packaging the second precursor by using PP melt-blown cloth to obtain the supported solid base deacidification and dewatering material. When the supported solid base deacidification and dewatering material is used, solid impurities can be effectively prevented from adhering to the surface to affect the activity, and the material loss can be effectively avoided, so that the deacidification and dewatering efficiency is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of deacidification and dehydration material preparation, in particular to a supported solid base deacidification and dehydration material and a preparation method thereof. BACKGROUND

[0002] The main components of the electrolyte include electrolyte salt, organic solvent and additive. Taking lithium ion battery as an example, the electrolyte salt usually adopts lithium hexafluorophosphate, and the lithium hexafluorophosphate has certain moisture sensitivity and can react with water to generate hydrogen fluoride and other acidic substances, so that the lithium hexafluorophosphate raw material contains certain hydrogen fluoride. The organic solvent includes carbonate solvents, carboxylic acid ester solvents and ether solvents, etc. Some water and hydroxyl-containing compounds may exist in these solvents. Therefore, in the production process of the electrolyte, in addition to directly bringing in hydrogen fluoride, the raw materials used also bring in water and hydroxyl-containing compounds. The reaction of these water and hydroxyl-containing compounds with lithium hexafluorophosphate can further generate hydrogen fluoride and other acidic substances. These acidic substances can corrode the pole piece in the battery cycle process, causing the battery life to be reduced and even causing safety accidents. Therefore, the water content and acid value of the electrolyte must be strictly controlled. However, in the actual production process, only management methods such as improving the raw material standard, molecular sieve dehydration and temperature control can be used for control. Once the product with unqualified acid value appears, it can only be treated as waste, which is neither environmentally friendly nor economical.

[0003] At present, there are also some existing technologies for deacidification and dehydration using MgO as an adsorbent. MgO is widely used as a solid base due to its high deacidification efficiency, low cost, easy availability, stable deacidification product, insolubility in organic solvents and strong anti-loss ability. However, in the process of deacidification and dehydration of the existing MgO solid base adsorbent, with the continuous reaction of acid and water with MgO, the generated Mg(OH)2 or salt impurities adhere to the 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 problems existing in the prior art. SUMMARY

[0004] The purpose of the present application is to provide a supported solid base deacidification and dehydration material and a preparation method thereof. The supported solid base deacidification and dehydration material can effectively avoid the adhesion 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-mentioned purpose, the present application provides a preparation method of a supported solid base deacidification and dehydration material, which comprises the following steps:

[0006] (1) mixing γ-alumina, magnesium hydroxide and starch to obtain dry mixture;

[0007] (2) adding acid solvent and alcohol solvent to the dry mixture to perform secondary kneading to obtain a wet mixture;

[0008] (3) performing extrusion granulation, drying and calcination on the wet mixture to obtain a first precursor;

[0009] (4) grinding and mixing calcium carbide and the first precursor to obtain a second precursor, and the mass ratio of the calcium carbide and the first precursor is 0.5-50:100;

[0010] (5) packaging the second precursor by using a PP melt-blown cloth to obtain a supported solid base deacidification and dehydration material.

[0011] Compared with the prior art, the present application has at least the following beneficial effects:

[0012] (1) In the present application, magnesium hydroxide is supported on gamma-alumina by kneading method and using starch as a binder, which improves the bonding strength between materials, and then a first precursor containing magnesium oxide solid base is generated by calcination, and calcium carbide is introduced into the first precursor to obtain a second precursor. The calcium carbide can react with acid and water to produce gas, thereby disturbing the interface, which can effectively prevent the generated magnesium hydroxide or salt impurities from adhering to the surface, maintain the interface activity, and thus effectively improve the dehydration and deacidification efficiency of the supported solid base deacidification and dehydration material.

[0013] (2) In the present application, acid solvent and alcohol solvent are used to perform secondary kneading on the dry mixture, which is helpful for further mixing of raw materials and facilitates subsequent extrusion granulation molding. At the same time, the acid solvent and alcohol solvent contained therein decompose or volatilize to release gas during the calcination process, thereby playing a pore-forming effect, improving the specific surface area of the material, and thus effectively improving the contact area of the material with acid and water, which is helpful for improving the deacidification and dehydration efficiency.

[0014] (3) In the present application, the second precursor is packaged by using a PP melt-blown cloth. The PP melt-blown cloth has many voids and a fluffy structure, which can play a good filtering effect and effectively prevent the loss of the material, thereby ensuring the deacidification and dehydration efficiency.

[0015] In summary, the supported solid base deacidification and dehydration material prepared by the preparation method of the present application can effectively prevent the generated impurities from being loaded on the surface thereof, and can effectively prevent the loss of the material, thereby improving the dehydration and deacidification efficiency.

[0016] Further, the mass ratio of the gamma-alumina, the magnesium hydroxide and the starch is 1000:100-300:1.

[0017] Further, the first kneading and the second kneading are both performed in a kneader.

[0018] Further, the time of the first kneading is 5 min to 240 min, and the rotation speed is 0 rpm to 120 rpm.

[0019] Further, the time of the second kneading is 5 min to 120 min, and the rotation speed is 5 rpm to 100 rpm.

[0020] Further, the acid solvent is at least one selected from nitric acid and acetic acid.

[0021] Further, the alcohol solvent is at least one selected from ethylene glycol and glycerol.

[0022] Further, the mass ratio of the dry mixture, the acid solvent and the alcohol solvent is 1000:50 to 300:1 to 100.

[0023] Further, the extrusion granulation is performed 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.

[0024] Further, the drying temperature is 50 DEG C to 110 DEG C, and the drying time is 6 h to 24 h.

[0025] Further, the calcination temperature is 400 DEG C to 580 DEG C, and the calcination time is 1 h to 4 h.

[0026] Further, the particle size Dv50 of the second precursor is 0.01 mm to 3 mm.

[0027] Another aspect of the present application provides a supported solid base deacidification and dehydration material, which is prepared by the above-mentioned preparation method of the supported solid base deacidification and dehydration material. BRIEF DESCRIPTION OF DRAWINGS

[0028] Figure 1 The supported solid base deacidification and dehydration material prepared in Example 1 of the present application. DETAILED DESCRIPTION

[0029] The preparation method of the supported solid base deacidification and dehydration material of the present application comprises the following steps:

[0030] (1) first kneading γ-alumina, magnesium hydroxide and starch to obtain a dry mixture;

[0031] (2) adding an acid solvent and an alcohol solvent to the dry mixture to perform second kneading to obtain a wet mixture;

[0032] (3) performing extrusion granulation, drying and calcination on the wet mixture to obtain a first precursor;

[0033] (4) grinding and mixing calcium carbide and the first precursor to obtain a second precursor.

[0034] (5) The second precursor is packaged by PP melt-blown cloth to obtain a supported solid base deacidification and dewatering material.

[0035] In step (1), the mass ratio of γ-alumina, magnesium hydroxide and starch is 1000:100~300:1. In some embodiments, the mass ratio of γ-alumina, magnesium hydroxide and starch is 1000:100:1, in some embodiments, the mass ratio of γ-alumina, magnesium hydroxide and starch is 1000:136:1, in some embodiments, the mass ratio of γ-alumina, magnesium hydroxide and starch is 1000:300:1. For example, the mass ratio of γ-alumina, 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 5min~240min. For example, the time of the first kneading can be, but is not limited to, 5min, 10min, 20min, 30min, 50min, 80min, 100min, 120min, 140min, 160min, 180min, 200min, 220min, 240min. The rotation speed is 0rpm~120rpm. For example, the rotation speed of the first kneading can be, but is not limited to, 0rpm, 10rpm, 20rpm, 40rpm, 60rpm, 80rpm, 100rpm, 120rpm. The magnesium hydroxide is a raw material for preparing magnesium oxide solid base. Preferably, the magnesium hydroxide of the present application is high-purity magnesium hydroxide. The γ-alumina is an inorganic compound with high thermal stability and excellent mechanical properties, which has high specific surface area and good pore structure. In the present application, the magnesium hydroxide is loaded on the γ-alumina matrix by kneading method, and the starch is used as a binder to improve the strength of the overall material structure.

[0036] 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 selected from nitric acid with a mass percentage of 20% to 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 mixture, the acid solvent, and the alcohol solvent is 1000:50 to 300:1 to 100. In some embodiments, the mass ratio of the dry mixture, the acid solvent, and the alcohol solvent is 1000:80 to 260:10 to 80. For example, but not limited to, the mass ratio of the dry mixture, the acid solvent, and the alcohol solvent can be 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 the alcohol solvent can further mix the raw materials, facilitating subsequent extrusion granulation molding. At the same time, the acid solvent can react with magnesium hydroxide to produce magnesium salt, which will decompose during calcination to obtain magnesium oxide with higher activity. The alcohol solvent and the unreacted acid solvent will decompose or volatilize during calcination, thereby playing a pore-forming effect on the material, increasing the specific surface area of the material, and effectively increasing the contact area of the solid alkali material with acid and water, thereby improving the deacidification and dehydration effect. The secondary kneading can be performed in a kneader, and the secondary kneading time is 5 min to 120 min. For example, but not limited to, the secondary kneading time can be 5 min, 10 min, 20 min, 30 min, 50 min, 80 min, 100 min, or 120 min. The secondary kneading speed is 5 rpm to 100 rpm. For example, but not limited to, the secondary kneading speed can be 5 rpm, 10 rpm, 20 rpm, 30 rpm, 40 rpm, 50 rpm, 60 rpm, 70 rpm, 80 rpm, 90 rpm, or 100 rpm.

[0037] In step (3), the extrusion granulation is performed in a screw extruder. The wet mixture is fed into the screw extruder for extrusion to obtain a strip with a diameter of 3-5 mm. The strip is cut into a material with a length of 0.5-10 cm. The material is then dried. The drying can be performed in an oven. The drying temperature is 50-110°C. For example, the drying temperature can be but is not limited to 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, or 110°C. The drying time is 6-24 h. For 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, or 24 h. The calcination can be performed in a muffle furnace. The calcination temperature is 400-580°C. For 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, or 580°C. The calcination time is 1-4 h. For example, the calcination time can be but is not limited to 1 h, 2 h, 3 h, or 4 h. During the temperature rising calcination, the acidic solvent contained in the wet mixture reacts with magnesium hydroxide to form a magnesium salt. At the same time, as the temperature rises, the alcohol solvent and the unreacted acidic solvent are decomposed or volatilized to form pores on the surface of the material, thereby increasing the specific surface area of the material and improving the adsorption treatment effect. Furthermore, the magnesium hydroxide and the magnesium salt are further decomposed at the calcination temperature to obtain solid alkali magnesium oxide.

[0038] In step (4), the mass ratio of calcium carbide and the first precursor is 0.5-50:100, in some embodiments, the mass ratio of calcium carbide and the first precursor is 0.5-30:100, and in some embodiments, the mass ratio of calcium carbide and the first precursor is 1-10:100. For example, the mass ratio of calcium carbide and 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, or 50:100. The grinding and mixing can be performed in a ball mill with a nitrogen atmosphere. After grinding and mixing, the particle size Dv50 of the second precursor can be 0.01 mm-3 mm. For 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, or 3 mm. Calcium carbide can react with acid and water to produce gas, thereby disturbing the interface. This can effectively prevent magnesium hydroxide or salt impurities generated during the adsorption process of solid base on acid or water from adhering to the surface of the solid base, maintain the interface activity, and achieve better dehydration and deacidification effect. 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 is helpful to further improve the deacidification and dehydration efficiency of the material.

[0039] In step (5), the PP melt-blown cloth has a large number of voids, a fluffy structure, good wrinkle resistance, and good filtering and shielding properties. The second precursor is packaged with the PP melt-blown cloth, which can achieve good filtering effect and effectively prevent material loss. The volume of the PP melt-blown cloth can be 50 mL, 60 mL, 70 mL, 80 mL, 90 mL, 100 mL, or 200 mL, but is not limited thereto.

[0040] The application also provides a supported solid base deacidification and dehydration material prepared by the above method.

[0041] To better illustrate the purpose, technical solutions and beneficial effects of the application, the application will be further described below with reference to specific examples. It should be noted that the following method is a further explanation of the application and should not be regarded as a limitation of the application.

[0042] Example 1

[0043] This example is a method for preparing a supported solid base deacidification and dehydration material, which comprises the following steps:

[0044] (1) first kneading γ-alumina, magnesium hydroxide and starch to obtain dry mixture, wherein the mass ratio of γ-alumina, magnesium hydroxide and starch is 1000:136:1, the first kneading is carried out in a kneader, the first kneading time is 5 min, and the rotating speed is 50 rpm;

[0045] (2) second kneading the dry mixture by adding acid solvent and alcohol solvent to obtain wet mixture, wherein the mass ratio of dry mixture, acid solvent and alcohol solvent is 1000:100:10, the acid solvent is selected from nitric acid (25% in mass), the alcohol solvent is selected from ethylene glycol, the second kneading is carried out in a kneader, the second kneading time is 60 min, and the rotating speed is 50 rpm;

[0046] (3) extruding the wet mixture by a screw extruder to obtain a strip with a diameter of 4 mm, cutting the strip into a material with a length of 10 cm, drying the material at 110°C for 24 h, and calcining the material at 580°C for 4 h to obtain a first precursor;

[0047] (4) grinding and mixing calcium carbide and the first precursor according to a mass ratio of 5:100 to obtain a second precursor with a particle size Dv50 of 1 mm;

[0048] (5) packaging the second precursor by using a 50 mL PP melt-blown cloth to obtain a volume of 50 mL of a supported solid base deacidification and dehydration material, as shown in Figure 1 .

[0049] Example 2

[0050] The embodiment is a preparation method of a supported solid base deacidification and dehydration material, comprising the following steps:

[0051] (1) first kneading γ-alumina, magnesium hydroxide and starch to obtain dry mixture, wherein the mass ratio of γ-alumina, magnesium hydroxide and starch is 1000:300:1, the first kneading is carried out in a kneader, the first kneading time is 5 min, and the rotating speed is 50 rpm;

[0052] (2) second kneading the dry mixture by adding acid solvent and alcohol solvent to obtain wet mixture, wherein the mass ratio of dry mixture, acid solvent and alcohol solvent is 1000:100:10, the acid solvent is selected from nitric acid (25% in mass), the alcohol solvent is selected from ethylene glycol, the second kneading is carried out in a kneader, the second kneading time is 60 min, and the rotating speed is 50 rpm;

[0053] (3) extruding the wet mixture by a screw extruder to obtain a strip with a diameter of 5 mm, cutting the strip into a material with a length of 10 cm, drying the material at 110°C for 24 h, and calcining the material at 580°C for 4 h to obtain a first precursor;

[0054] (4) the second precursor with a particle size Dv50 of 1 mm is obtained by grinding and mixing calcium carbide and the first precursor at a mass ratio of 5:100;

[0055] (5) the second precursor is packaged by using a 50 mL PP melt-blown cloth to obtain a 50 mL volume of the supported solid base deacidification and dehydration material.

[0056] Example 3

[0057] The embodiment is a preparation method of a supported solid base deacidification and dehydration material, comprising the steps of:

[0058] (1) dry mixture is obtained by primary kneading of γ-alumina, magnesium hydroxide and starch, wherein the mass ratio of γ-alumina, magnesium hydroxide and starch is 1000:220:1, the primary kneading is performed in a kneader, the primary kneading time is 10 min, and the rotation speed is 100 rpm;

[0059] (2) wet mixture is obtained by secondary kneading of the dry mixture, acid solvent and alcohol solvent, wherein the mass ratio of the dry mixture, acid solvent and alcohol solvent is 1000:300:100, the acid solvent is selected from acetic acid, the alcohol solvent is selected from glycerol, the secondary kneading is performed in a kneader, the secondary kneading time is 30 min, and the rotation speed is 80 rpm;

[0060] (3) the wet mixture is extruded by a screw extruder to obtain a strip with a diameter of 5 mm, the strip is cut into a material with a length of 5 cm, the material is dried at 70°C for 24 h, and then calcined at 500°C for 4 h to obtain the first precursor;

[0061] (4) the second precursor with a particle size Dv50 of 3 mm is obtained by grinding and mixing calcium carbide and the first precursor at a mass ratio of 10:100;

[0062] (5) the second precursor is packaged by using a 50 mL PP melt-blown cloth to obtain a 50 mL volume of the supported solid base deacidification and dehydration material.

[0063] Comparative Example 1

[0064] The embodiment is a preparation method of a supported solid base deacidification and dehydration material, comprising the steps of:

[0065] (1) dry mixture is obtained by primary kneading of γ-alumina, magnesium hydroxide and starch, wherein the mass ratio of γ-alumina, magnesium hydroxide and starch is 1000:136:1, the primary kneading is performed in a kneader, the primary kneading time is 5 min, and the rotation speed is 50 rpm;

[0066] (2) adding an acid solvent and an alcohol solvent into the dry mixture to perform secondary kneading to obtain a wet mixture, wherein 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 (25% by mass), and the alcohol solvent is selected from ethylene glycol, the secondary kneading is performed in a kneader, the secondary kneading time is 60 min, and the rotation speed is 50 rpm;

[0067] (3) extruding the wet mixture through a screw extruder to obtain a strip-shaped material with a diameter of 4 mm, cutting the strip-shaped material into a material with a length of 10 cm, drying the material at 110°C for 24 h, and calcining the material at 580°C for 4 h to obtain a first precursor;

[0068] (4) grinding the first precursor to obtain a second precursor with a particle size Dv50 of 1 mm;

[0069] (5) packaging the second precursor by using a 50 mL PP melt-blown cloth to obtain a 50 mL volume of the supported solid base deacidification and dehydration material.

[0070] Comparative Example 2

[0071] The present comparative example is a preparation method of a supported solid base deacidification and dehydration material, comprising the following steps:

[0072] (1) performing primary kneading on γ-alumina, magnesium hydroxide and starch to obtain a dry mixture, wherein the mass ratio of the γ-alumina, the magnesium hydroxide and the starch is 1000:136:1, the primary kneading is performed in a kneader, the primary kneading time is 5 min, and the rotation speed is 50 rpm;

[0073] (2) adding an acid solvent and an alcohol solvent into the dry mixture to perform secondary kneading to obtain a wet mixture, wherein 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 (25% by mass), and the alcohol solvent is selected from ethylene glycol, the secondary kneading is performed in a kneader, the secondary kneading time is 60 min, and the rotation speed is 50 rpm;

[0074] (3) extruding the wet mixture through a screw extruder to obtain a strip-shaped material with a diameter of 4 mm, cutting the strip-shaped material into a material with a length of 10 cm, drying the material at 110°C for 24 h, and calcining the material at 580°C for 4 h to obtain a first precursor;

[0075] (4) grinding and mixing calcium carbide and the first precursor at a mass ratio of 0.3:100 to obtain a second precursor with a particle size Dv50 of 1 mm;

[0076] (5) packaging the second precursor by using a 50 mL PP melt-blown cloth to obtain a 50 mL volume of the supported solid base deacidification and dehydration material.

[0077] Comparative Example 3

[0078] The present comparative example is a preparation method of a supported solid base deacidification and dehydration material, comprising the steps of:

[0079] (1) a dry mixture was obtained by one-time kneading of γ-alumina, magnesium hydroxide and starch, wherein the mass ratio of γ-alumina, magnesium hydroxide and starch was 1000:136:1, the one-time kneading was carried out in a kneader, the one-time kneading time was 5 min, and the rotation speed was 50 rpm;

[0080] (2) a wet mixture was obtained by adding an alcohol solvent to the dry mixture for secondary kneading, wherein 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 secondary kneading time was 60 min, and the rotation speed was 50 rpm;

[0081] (3) a strip-shaped material with a diameter of 4 mm was obtained by extruding the wet mixture through a screw extruder, the strip-shaped material was cut into a material with a length of 10 cm, the material was dried at 110°C for 24 h, and then calcined at 580°C for 4 h to obtain a first precursor;

[0082] (4) a second precursor with a particle size Dv50 of 1 mm was obtained by grinding and mixing calcium carbide and the first precursor at a mass ratio of 5:100;

[0083] (5) the second precursor was packaged using a 50 mL PP melt-blown cloth to obtain a supported solid base deacidification and dehydration material with a volume of 50 mL.

[0084] Comparative Example 4

[0085] The present comparative example is a preparation method of a supported solid base deacidification and dehydration material, comprising the steps of:

[0086] (1) a dry mixture was obtained by one-time kneading of γ-alumina, magnesium hydroxide and starch, wherein the mass ratio of γ-alumina, magnesium hydroxide and starch was 1000:136:1, the one-time kneading was carried out in a kneader, the one-time kneading time was 5 min, and the rotation speed was 50 rpm;

[0087] (2) a wet mixture was obtained by adding an alcohol solvent to the dry mixture for secondary kneading, wherein the mass ratio of the dry mixture 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 secondary kneading time was 60 min, and the rotation speed was 50 rpm;

[0088] (3) a strip-shaped material with a diameter of 4 mm was obtained by extruding the wet mixture through a screw extruder, the strip-shaped material was cut into a material with a length of 10 cm, the material was dried at 110°C for 24 h, and then calcined at 580°C for 4 h to obtain a first precursor;

[0089] (4) The second precursor with a particle size Dv50 of 1 mm, i.e., the supported solid base deacidification and dewatering material, is obtained by grinding and mixing calcium carbide and the first precursor at a mass ratio of 5:100.

[0090] The supported solid base deacidification and dewatering materials with a volume of 50 mL (dry weight of 41.00 g) prepared in Examples 1-3 and Comparative Examples 1-4 are respectively placed in a stainless steel fixed bed with an inner diameter of 20 cm, electrolyte is introduced, and the flow rate of the electrolyte is controlled at 5 m 3 / h (the acid value of the electrolyte is 140 ppm, the moisture is 35 ppm, and the total volume is 20 L), and finally the acid value and moisture of the deacidified and dewatered electrolyte are analyzed, and the supported solid base deacidification and dewatering materials of each example and comparative example are weighed after being dried in a vacuum drying oven at 35°C for 24 h, and the analysis test results are shown in Table 1.

[0091] Table 1 Analysis test results of Examples 1-3 and Comparative Examples 1-4

[0092]

[0093] For details, see the analysis results in Table 1. As can be seen from the analysis results of Examples 1-3 and Comparative Examples 1-4, the supported solid base deacidification and dewatering material prepared by the preparation method of the present application has a more excellent deacidification and dewatering effect.

[0094] Further comparison of the results of Example 1 and Comparative Examples 1-2 shows that when calcium carbide is absent or the amount of calcium carbide added is less than the range of the present application, the deacidification and dewatering effect is affected, indicating that the addition of a certain amount of calcium carbide is beneficial to improving the deacidification and dewatering performance of the supported solid base deacidification and dewatering material of the present application. As can be seen from the analysis results of Example 1 and Comparative Examples 3-4, when the acid solvent is replaced by water, the deacidification and dewatering effect of the solid base is significantly affected; when the second precursor is not packaged, the solid base deacidification and dewatering material is lost seriously, and thus the deacidification and dewatering effect is reduced to a certain extent.

[0095] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application and are not intended to limit the scope of protection of the present application. Although the present application has been described in detail with reference to the preferred embodiments, it is not limited to the examples listed in the embodiments. Those skilled in the art should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present application.

Claims

1. A method for producing a supported solid base deacidification and dehydration material, characterized by, The method comprises the steps of: (1) mixing γ-alumina, magnesium hydroxide and starch to obtain dry mixture; (2) adding acid solvent and alcohol solvent to the dry mixture to obtain wet mixture, wherein the acid solvent is at least one selected from nitric acid and acetic acid, and the alcohol solvent is at least one selected from ethylene glycol and glycerol; (3) extruding, drying and calcining the wet mixture to obtain first precursor; (4) grinding and mixing calcium carbide and the first precursor to obtain second precursor, wherein the mass ratio of calcium carbide to the first precursor is 0.5-50:100; (5) packaging the second precursor by using PP melt-blown cloth to obtain supported solid base deacidification and dehydration material.

2. The method for preparing a supported solid base deacidifying and dehydrating material according to claim 1, characterized by, 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 deacidifying and dehydrating material according to claim 1, characterized by, The first mixing and the second mixing are both carried out in a kneader, the first mixing is carried out for 5-240 min at a rotation speed of 0-120 rpm, and the second mixing is carried out for 5-120 min at a rotation speed of 5-100 rpm.

4. The method for preparing a supported solid base deacidifying and dehydrating material according to claim 1, characterized by, The mass ratio of the dry mixture, the acid solvent and the alcohol solvent is 1000:50-300:1-100.

5. The method for preparing a supported solid base deacidifying and dehydrating material according to claim 1, characterized by, The extrusion granulation is carried out in a screw extruder, and the diameter of the material obtained after the extrusion granulation is 3-5 mm, and the length is 0.5-10 cm.

6. The method for preparing a supported solid base deacidifying and dehydrating material according to claim 1, characterized by, The drying is carried out at a temperature of 50-110 ℃ for 6-24 h.

7. The method for preparing a supported solid base deacidifying and dehydrating material according to claim 1, characterized by, The calcination is carried out at a temperature of 400-580 ℃ for 1-4 h.

8. The method for preparing a supported solid base deacidifying and dehydrating material according to claim 1, characterized by, The particle size Dv50 of the second precursor is 0.01-3 mm.

9. A supported solid base deacidification and dehydration material, characterized by, The supported solid base deacidification and dehydration material is prepared by using the preparation method of any one of claims 1-8.

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