Preparation method of tensile plant-based cobalt salt
By using arachid acid, cobalt hydroxide, ethyl 3-ethoxypropionate and plant microcrystalline cellulose as raw materials, the tensile-resistant plant-based cobalt salts are solved, the environmentally unfriendly problem of organic solvents is improved, the performance of rubber products is achieved and sustainable development is achieved.
Patent Information
- Application Number
- CN202510445577.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-10
- Publication Date
- 2025-08-05
AI Technical Summary
The organic solvents used in the existing cobalt salt synthesis process are uneconomical and affect the aging resistance of rubber cords. The synthesis process has high energy consumption and is difficult to completely recycle, resulting in environmental pollution.
Arachid acid, cobalt hydroxide, ethyl 3-ethoxypropionate and plant microcrystalline cellulose are used as raw materials to prepare tensile-resistant plant-based cobalt salts through specific stirring, heating, distillation and granulation processes. The environmentally friendly solvent ethyl 3-ethoxypropionate is used, and active functional groups are introduced to improve performance.
The prepared plant-based cobalt salt has good oxidation resistance and corrosion resistance, which improves the performance of rubber products, while reducing environmental pollution and achieving sustainable development.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of preparation of plant-based cobalt salts, and in particular relates to a method for preparing tensile-resistant plant-based cobalt salts. Background Art
[0002] The cobalt boroacylate and cobalt neodecanoate in the existing technology are mostly mixed carboxylic acids mainly composed of medium and short chain acids. The acid radical acidity of the cobalt salt is relatively strong, which affects the aging resistance of the steel cord. In addition, Co3+ is easily generated during the synthesis process. Co3+ is not conducive to rubber adhesion and cannot promote the formation of the rubber cord bonding layer. In addition, most synthesis technologies use non-environmentally friendly (benzene) solvents. The use of organic solvents will have the following defects: 1. Melting crystalline organic acids in the early stage of the reaction will increase energy consumption. 2. The storage of organic solvents has stricter environmental requirements and poses certain safety hazards. 3. After use, the organic solvent needs to be recycled. The process flow of the recycling process varies in complexity, but it will consume energy resources. If it cannot be completely recycled, some reagents will inevitably be discharged into the environmental system. For this reason, we propose a preparation method for tensile-resistant plant-based cobalt salts. Summary of the Invention
[0003] The present invention provides a method for preparing a tensile-resistant plant-based cobalt salt to solve the problems raised in the above background technology.
[0004] To achieve the above object, the present invention provides the following technical solution: a method for preparing a tensile-resistant plant-based cobalt salt, comprising the following steps:
[0005] S1. Prepare raw materials: 55-65 parts of arachidic acid, 10-15 parts of cobalt hydroxide, 25-35 parts of ethyl 3-ethoxypropionate, and 5-10 parts of plant microcrystalline cellulose;
[0006] S2. Raw material pretreatment:
[0007] Arachidic acid: The arachidic acid is filtered to remove possible tiny solid impurities, and then the arachidic acid is preheated to reduce the viscosity of the arachidic acid;
[0008] Cobalt hydroxide: grinding it to make its particle size distribution between 5μm and 15μm;
[0009] Ethyl 3-ethoxypropionate: Test to ensure that its acid value is within the range of 0.01mgKOH / g to 0.05mgKOH / g and its base value is within the range of 0.005mgKOH / g to 0.02mgKOH / g;
[0010] Plant microcrystalline cellulose: Dry it in a vacuum drying oven until the moisture content is less than 0.3%. During the drying process, control the drying temperature at 50℃~60℃;
[0011] S3, adding ethyl 3-ethoxypropionate to the reactor, so that ethyl 3-ethoxypropionate serves as the solvent of the entire reaction system;
[0012] S4. Add arachidic acid and solvent to the reactor and stir for 5 minutes. The stirring speed is initially 100 rpm to 150 rpm, gradually increased to 200 rpm to 250 rpm after stirring for 1 to 2 minutes, and finally maintained at 300 rpm to 350 rpm at the end of the 5-minute stirring.
[0013] S5, add cobalt hydroxide and mix, stir at room temperature for 30 minutes, then raise the temperature to 90°C to 100°C, and maintain the temperature for reflux reaction for 1 hour to 2 hours;
[0014] S6. Heat to 175°C to 185°C and distill for 1.5 hours at a negative pressure of ≤-0.085 MPa, removing wastewater and solvent. During the 1.5-hour distillation, precisely control the temperature fluctuation to within ±1°C and the pressure fluctuation to within ±0.005 MPa.
[0015] S7. Add plant microcrystalline cellulose, stir for 1 hour, and then granulate.
[0016] Furthermore, in step S2, the eicosanoid is filtered using a filter membrane with a pore size of 0.1 μm to 0.2 μm, and the eicosanoid is preheated to 30° C. to 40° C. before being added to the reactor;
[0017] Cobalt hydroxide: Detect the moisture content in cobalt hydroxide and control the moisture content below 0.5%;
[0018] Plant microcrystalline cellulose: The dried plant microcrystalline cellulose is subjected to surface activation treatment, and plasma treatment technology is used to introduce active functional groups, such as hydroxyl or carboxyl groups, on its surface.
[0019] Furthermore, in step S3, ethyl 3-ethoxypropionate is added to the reactor by dropwise addition, and the dropwise addition speed is controlled at 1 mL / min to 2 mL / min. During the dropwise addition of the solvent, stirring is performed at a stirring speed of 50 r / min to 100 r / min.
[0020] Before the dropwise addition of ethyl 3-ethoxypropionate, ethyl 3-ethoxypropionate was preheated to a temperature within ±5° C. relative to the temperature in the reactor.
[0021] Furthermore, in step S4, arachidic acid is slowly added into the reactor containing the solvent in a thin stream, and ultrasonic wave is used to assist dispersion, and the power of the ultrasonic wave is set to 100W to 200W.
[0022] Furthermore, in step S5, before adding cobalt hydroxide, cobalt hydroxide is premixed with a small amount of ethyl 3-ethoxypropionate, and then the mixture of cobalt hydroxide and ethyl 3-ethoxypropionate is added to the reactor in batches.
[0023] Furthermore, the stirring speed of the premixed mixture of the cobalt hydroxide and a small amount of ethyl 3-ethoxypropionate is 300 r / min to 400 r / min, the stirring time is 5 min to 10 min, and the mixture of cobalt hydroxide and ethyl 3-ethoxypropionate is added to the reactor in 3 to 5 batches, with an addition interval of 2 min to 3 min for each batch.
[0024] Furthermore, in step S6, before the distillation operation is performed, the distillation apparatus is checked for air tightness to ensure that the system is leak-free. At the same time, the distillation apparatus is preheated, and components such as the distillation flask and the condenser are preheated to 150°C to 160°C.
[0025] Furthermore, in step S7, when adding plant microcrystalline cellulose, it is evenly sprinkled on the surface of the reaction system and then slowly stirred. The stirring speed is initially 100 r / min to 150 r / min, and as the plant microcrystalline cellulose is continuously added, the stirring speed is gradually increased to 200 r / min to 250 r / min.
[0026] The beneficial effects of the present invention are:
[0027] 1. This invention is based on plant-based cobalt carboxylate salts. Its plant-based raw material, arachidic acid, is a natural organic compound and a saturated fatty acid found in peanuts, vegetables, and fish oils. It can be produced by hydrolyzing and separating peanut oil. Arachidic acid is a C20 acid with minimal acidic side effects, high purity, and antioxidant properties, which can improve the thermal and oxidative aging resistance and corrosion resistance of rubber products.
[0028] 2. The solvent added in the present invention is 3-ethoxyethyl propionate, which has good biodegradability and renewability and can be recycled as a solvent without producing additional byproducts. The use of ester products can reduce dependence on non-renewable resources, thereby helping to protect the environment and ecosystem. As a sustainable development alternative, environmentally friendly ester products will become the mainstream of the future. They are not only environmentally friendly but also can promote sustainable economic and social development. The preparation process of the present invention is gentle, and the melting point of the cobalt salt produced is moderate, making granulation, transportation, and use convenient.
[0029] 3. The plant microcrystalline cellulose added in the preparation process of the present invention is present in large quantities in plants, animals and microorganisms. Straw, bagasse, textiles made from wood, cotton, etc., paper, etc. also contain a large amount of cellulose. It has the advantages of wide availability, low cost, renewable, degradable, environmentally friendly and low density. It improves the mechanical properties and cross-linking density of rubber, and improves the water absorption performance, barrier performance, conductivity and dynamic mechanical properties. After addition, the water aging resistance and vulcanization adhesion performance of cobalt salt are improved. DETAILED DESCRIPTION
[0030] Example 1:
[0031] A method for preparing a tensile-resistant plant-based cobalt salt comprises the following steps:
[0032] Raw materials preparation: arachidic acid: 38 parts, cobalt hydroxide: 15 parts, ethyl 3-ethoxypropionate: 25 parts and plant microcrystalline cellulose: 5 parts;
[0033] Arachidic acid: purity ≥99%, acid value: 170~190mgKOH / g;
[0034] Cobalt hydroxide: industrial cobalt hydroxide with a cobalt content of ≥61.5%;
[0035] Ethyl 3-ethoxypropionate: industrial ethyl 3-ethoxypropionate, purity ≥99%;
[0036] Plant microcrystalline cellulose: industrial plant microcrystalline cellulose, active ingredient ≥99%;
[0037] S2. Arachidic acid: Filter the arachidic acid using a filter membrane with a pore size of 0.1 μm to 0.2 μm to remove any possible tiny solid impurities. Then, preheat the arachidic acid to reduce its viscosity. The arachidic acid is preheated to 30° C. to 40° C. before being added to the reactor.
[0038] Cobalt hydroxide: First, test the moisture content of cobalt hydroxide and control it to below 0.5%. Then grind it to a particle size distribution between 5μm and 15μm.
[0039] Ethyl 3-ethoxypropionate: Test to ensure that its acid value is within the range of 0.01mgKOH / g to 0.05mgKOH / g and its base value is within the range of 0.005mgKOH / g to 0.02mgKOH / g;
[0040] Plant microcrystalline cellulose: Dry it in a vacuum drying oven until the moisture content is less than 0.3%. During the drying process, the drying temperature is controlled at 50℃ to 60℃. The dried plant microcrystalline cellulose is subjected to surface activation treatment. Plasma treatment technology is used to introduce active functional groups, such as hydroxyl or carboxyl groups, on its surface.
[0041] S3, adding ethyl 3-ethoxypropionate to the reactor, making ethyl 3-ethoxypropionate as the solvent of the entire reaction system, ethyl 3-ethoxypropionate is added to the reactor by dropwise addition, and the dropwise addition speed is controlled at 1 mL / min to 2 mL / min. During the dropwise addition of the solvent, stirring is performed at a stirring speed of 50 r / min to 100 r / min;
[0042] Before adding ethyl 3-ethoxypropionate dropwise, preheat the ethyl 3-ethoxypropionate to a temperature within ±5° C.
[0043] S4. Add arachidic acid and solvent to the reactor and stir for 5 minutes. The stirring speed is initially 100 r / min to 150 r / min, gradually increased to 200 r / min to 250 r / min after stirring for 1 to 2 minutes, and finally maintained at 300 r / min to 350 r / min at the end of the 5-minute stirring. Slowly add arachidic acid to the reactor containing the solvent in a thin stream, and use ultrasonic wave to assist dispersion. The ultrasonic wave power is set to 100 W to 200 W.
[0044] S5, add cobalt hydroxide and mix, stir at room temperature for 30min, then raise the temperature to 100°C, and maintain the temperature for reflux reaction for 2h, before adding cobalt hydroxide, premix the cobalt hydroxide with a small amount of ethyl 3-ethoxypropionate, then add the cobalt hydroxide and ethyl 3-ethoxypropionate mixture into the reactor in batches, the stirring speed of the premix of cobalt hydroxide and a small amount of ethyl 3-ethoxypropionate is 300r / min~400r / min, the stirring time is 5min~10min, and the cobalt hydroxide and ethyl 3-ethoxypropionate mixture is added into the reactor in 3~5 batches, and the addition interval of each batch is 2min~3min;
[0045] S6. During the distillation operation, perform an airtightness check on the distillation apparatus to ensure that there are no leaks in the system. Preheat the distillation apparatus by preheating the distillation flask, condenser and other components to 150°C to 160°C, then heat to 185°C, and distill for 2 hours under a negative pressure of ≤-0.085 MPa. Remove wastewater and solvent. During the 2-hour distillation process, accurately control the temperature fluctuation within ±1°C and the pressure fluctuation within ±0.005 MPa.
[0046] S7. Add plant microcrystalline cellulose, stir for 0.5 hours, and then discharge and granulate. Add plant microcrystalline cellulose at 180-185° C. When adding plant microcrystalline cellulose, sprinkle it evenly on the surface of the reaction system, and then stir slowly. The stirring speed is initially 100 r / min-150 r / min. As the plant microcrystalline cellulose is continuously added, the stirring speed is gradually increased to 200 r / min-250 r / min, thereby obtaining a reaction product with a cobalt content of 8.53%, a melting point of 88° C., and a reddish-purple solid appearance.
[0047] Example 2:
[0048] A method for preparing a tensile-resistant plant-based cobalt salt comprises the following steps:
[0049] Raw materials preparation: arachidic acid: 25 parts, cobalt hydroxide: 15 parts, ethyl 3-ethoxypropionate: 30 parts and plant microcrystalline cellulose: 5 parts;
[0050] Arachidic acid: purity ≥99%, acid value: 170~190mgKOH / g;
[0051] Cobalt hydroxide: industrial cobalt hydroxide with a cobalt content of ≥61.5%;
[0052] Ethyl 3-ethoxypropionate: industrial ethyl 3-ethoxypropionate, purity ≥99%;
[0053] Plant microcrystalline cellulose: industrial plant microcrystalline cellulose, active ingredient ≥99%;
[0054] S2. Arachidic acid: Filter the arachidic acid using a filter membrane with a pore size of 0.1 μm to 0.2 μm to remove any possible tiny solid impurities. Then, preheat the arachidic acid to reduce its viscosity. The arachidic acid is preheated to 30° C. to 40° C. before being added to the reactor.
[0055] Cobalt hydroxide: First, test the moisture content of the cobalt hydroxide and control it to below 0.5%. Then grind it to a particle size distribution between 5μm and 15μm.
[0056] Ethyl 3-ethoxypropionate: Test to ensure that its acid value is within the range of 0.01mgKOH / g to 0.05mgKOH / g and its base value is within the range of 0.005mgKOH / g to 0.02mgKOH / g;
[0057] Plant microcrystalline cellulose: Dry it in a vacuum drying oven until the moisture content is less than 0.3%. During the drying process, the drying temperature is controlled at 50℃ to 60℃. The dried plant microcrystalline cellulose is subjected to surface activation treatment. Plasma treatment technology is used to introduce active functional groups, such as hydroxyl or carboxyl groups, on its surface.
[0058] S3, adding ethyl 3-ethoxypropionate to the reactor, making ethyl 3-ethoxypropionate as the solvent of the entire reaction system, ethyl 3-ethoxypropionate is added to the reactor by dropwise addition, and the dropwise addition speed is controlled at 1 mL / min to 2 mL / min. During the dropwise addition of the solvent, stirring is performed at a stirring speed of 50 r / min to 100 r / min;
[0059] Before adding ethyl 3-ethoxypropionate dropwise, preheat the ethyl 3-ethoxypropionate to a temperature within ±5° C.
[0060] S4. Add arachidic acid and solvent to the reactor and stir for 5 minutes. The stirring speed is initially 100 r / min to 150 r / min, gradually increased to 200 r / min to 250 r / min after stirring for 1 to 2 minutes, and finally maintained at 300 r / min to 350 r / min at the end of the 5-minute stirring. Slowly add arachidic acid to the reactor containing the solvent in a thin stream, and use ultrasonic wave to assist dispersion. The ultrasonic wave power is set to 100 W to 200 W.
[0061] S5, add cobalt hydroxide and mix, stir at room temperature for 30min, then raise the temperature to 100°C, and maintain the temperature for reflux reaction for 1h, before adding cobalt hydroxide, premix the cobalt hydroxide with a small amount of ethyl 3-ethoxypropionate, then add the cobalt hydroxide and ethyl 3-ethoxypropionate mixture to the reactor in batches, the stirring speed of the premix of cobalt hydroxide and a small amount of ethyl 3-ethoxypropionate is 300r / min~400r / min, the stirring time is 5min~10min, and the cobalt hydroxide and ethyl 3-ethoxypropionate mixture is added to the reactor in 3~5 batches, and the addition interval of each batch is 2min~3min;
[0062] S6. During the distillation operation, perform an airtight check on the distillation apparatus to ensure that there are no leaks in the system. Preheat the distillation apparatus by preheating the distillation flask, condenser and other components to 150°C to 160°C, then heat to 185°C, and distill for 2 hours under a negative pressure of ≤-0.085 MPa. Remove wastewater and solvents. During the 2-hour distillation process, accurately control the temperature fluctuation within ±1°C and the pressure fluctuation within ±0.005 MPa.
[0063] S7. Add plant microcrystalline cellulose, stir for 0.5 hours, and then discharge and granulate. Add plant microcrystalline cellulose at 180-185° C. When adding plant microcrystalline cellulose, sprinkle it evenly on the surface of the reaction system, and then stir slowly. The stirring speed is initially 100 r / min-150 r / min. As the plant microcrystalline cellulose is continuously added, the stirring speed is gradually increased to 200 r / min-250 r / min, thereby obtaining a reaction product with a cobalt content of 8.49%, a melting point of 87° C., and a reddish-purple solid appearance.
[0064] Example 3:
[0065] A method for preparing a tensile-resistant plant-based cobalt salt comprises the following steps:
[0066] Raw materials preparation: arachidic acid: 26 parts, cobalt hydroxide: 13 parts, ethyl 3-ethoxypropionate: 25 parts and plant microcrystalline cellulose: 5 parts;
[0067] Arachidic acid: purity ≥99%, acid value: 170~190mgKOH / g;
[0068] Cobalt hydroxide: industrial cobalt hydroxide with a cobalt content of ≥61.5%;
[0069] Ethyl 3-ethoxypropionate: industrial ethyl 3-ethoxypropionate, purity ≥99%;
[0070] Plant microcrystalline cellulose: industrial plant microcrystalline cellulose, active ingredient ≥99%;
[0071] S2. Arachidic acid: Filter the arachidic acid using a filter membrane with a pore size of 0.1 μm to 0.2 μm to remove any possible tiny solid impurities. Then, preheat the arachidic acid to reduce its viscosity. The arachidic acid is preheated to 30° C. to 40° C. before being added to the reactor.
[0072] Cobalt hydroxide: First, test the moisture content of cobalt hydroxide and control it to below 0.5%. Then grind it to a particle size distribution between 5μm and 15μm.
[0073] Ethyl 3-ethoxypropionate: Test to ensure that its acid value is within the range of 0.01mgKOH / g to 0.05mgKOH / g and its base value is within the range of 0.005mgKOH / g to 0.02mgKOH / g;
[0074] Plant microcrystalline cellulose: Dry it in a vacuum drying oven until the moisture content is less than 0.3%. During the drying process, the drying temperature is controlled at 50℃ to 60℃. The dried plant microcrystalline cellulose is subjected to surface activation treatment. Plasma treatment technology is used to introduce active functional groups, such as hydroxyl or carboxyl groups, on its surface.
[0075] S3, adding ethyl 3-ethoxypropionate to the reactor, making ethyl 3-ethoxypropionate as the solvent of the entire reaction system, ethyl 3-ethoxypropionate is added to the reactor by dropwise addition, and the dropwise addition speed is controlled at 1 mL / min to 2 mL / min. During the dropwise addition of the solvent, stirring is performed at a stirring speed of 50 r / min to 100 r / min;
[0076] Before adding ethyl 3-ethoxypropionate dropwise, preheat the ethyl 3-ethoxypropionate to a temperature within ±5° C.
[0077] S4. Add arachidic acid and solvent to the reactor and stir for 5 minutes. The stirring speed is initially 100 r / min to 150 r / min, gradually increased to 200 r / min to 250 r / min after stirring for 1 to 2 minutes, and finally maintained at 300 r / min to 350 r / min at the end of the 5-minute stirring. Slowly add arachidic acid to the reactor containing the solvent in a thin stream, and use ultrasonic wave to assist dispersion. The ultrasonic wave power is set to 100 W to 200 W.
[0078] S5, add cobalt hydroxide and mix, stir at room temperature for 30min, then raise the temperature to 100°C, and maintain the temperature for reflux reaction for 2h, before adding cobalt hydroxide, premix the cobalt hydroxide with a small amount of ethyl 3-ethoxypropionate, then add the cobalt hydroxide and ethyl 3-ethoxypropionate mixture into the reactor in batches, the stirring speed of the premix of cobalt hydroxide and a small amount of ethyl 3-ethoxypropionate is 300r / min~400r / min, the stirring time is 5min~10min, and the cobalt hydroxide and ethyl 3-ethoxypropionate mixture is added into the reactor in 3~5 batches, and the addition interval of each batch is 2min~3min;
[0079] S6. During the distillation operation, perform an airtightness check on the distillation apparatus to ensure that there are no leaks in the system. Preheat the distillation apparatus by preheating the distillation flask, condenser and other components to 150°C to 160°C, then heat to 185°C, and distill for 3 hours under a negative pressure of ≤-0.085 MPa. Remove wastewater and solvents. During the 3-hour distillation process, accurately control the temperature fluctuation within ±1°C and the pressure fluctuation within ±0.005 MPa.
[0080] S7. Add plant microcrystalline cellulose, stir for 0.5 hours, and then discharge and granulate. Add plant microcrystalline cellulose at 180-185° C. When adding plant microcrystalline cellulose, sprinkle it evenly on the surface of the reaction system, and then stir slowly. The stirring speed is initially 100 r / min-150 r / min. As the plant microcrystalline cellulose is continuously added, the stirring speed is gradually increased to 200 r / min-250 r / min, thereby obtaining a reaction product with a cobalt content of 8.52%, a melting point of 87° C., and a reddish-purple solid appearance.
[0081] Table 1 shows the addition of cobalt salts, calculated so that the content of metallic cobalt in 100 parts of rubber hydrocarbon does not exceed 0.3 parts. The preparation method of the rubber compound adopts the existing conventional method.
[0082]
[0083]
[0084] Table 2 shows the mechanical properties test and vulcanization performance test of the above six groups of formula rubber samples according to the national standards GB / T329-2008, GB / T328-2009, and GB / T16584. The rubber physical properties sample preparation and vulcanization conditions are: 150℃*30min, rheological temperature 150℃*60min, and the test data.
[0085]
[0086] Table 3 shows the extraction force test and thermal oxidation aging (105°C for 3 days), salt water aging (5% NaCl solution for 7 days), and wet heat aging (93°C*95RH% for 7 days) of the above-mentioned formula samples with reference to GB-T 16586-1996. The initial vulcanization conditions are: 150°C*30min. Steel cord specifications: 3*0.20+6*0.35NT.
[0087]
[0088]
[0089] From the above examples, it can be seen that under the same conditions, the plant-based arachidic acid cobalt of the present invention is superior to ordinary carboxylic acid cobalt salts in terms of rubber attachment rate, extraction force, hot air aging performance and salt water aging performance after vulcanization of rubber and steel cord, and has excellent comprehensive mechanical properties. This shows that the arachidic acid cobalt prepared by the present invention has good adhesion promotion and antioxidant effects between metal and rubber, thereby improving various properties of rubber.
[0090] The above shows and describes 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 above embodiments and descriptions are merely preferred examples of the present invention and are not intended to limit the present invention. Various changes and improvements may be made to the present invention without departing from the spirit and scope of the present invention. Such changes and improvements fall within the scope of the present invention. The scope of protection claimed in the present invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing a tensile-resistant plant-based cobalt salt, characterized by: The following steps are involved: S1. Prepare raw materials: 55-65 parts of arachidic acid, 10-15 parts of cobalt hydroxide, 25-35 parts of ethyl 3-ethoxypropionate, and 5-10 parts of plant microcrystalline cellulose; S2. Raw material pretreatment: Arachidic acid: The arachidic acid is filtered to remove possible tiny solid impurities, and then the arachidic acid is preheated to reduce the viscosity of the arachidic acid; Cobalt hydroxide: grinding it to make its particle size distribution between 5μm and 15μm; Ethyl 3-ethoxypropionate: Test to ensure that its acid value is within the range of 0.01mgKOH / g to 0.05mgKOH / g and its base value is within the range of 0.005mgKOH / g to 0.02mgKOH / g; Plant microcrystalline cellulose: Dry it in a vacuum drying oven until the moisture content is less than 0.3%. During the drying process, control the drying temperature at 50℃~60℃; S3, adding ethyl 3-ethoxypropionate to the reactor, so that ethyl 3-ethoxypropionate serves as the solvent of the entire reaction system; S4. Add arachidic acid and solvent to the reactor and stir for 5 minutes. The stirring speed is initially 100 rpm to 150 rpm, gradually increased to 200 rpm to 250 rpm after stirring for 1 to 2 minutes, and finally maintained at 300 rpm to 350 rpm at the end of the 5-minute stirring. S5, add cobalt hydroxide and mix, stir at room temperature for 30 minutes, then raise the temperature to 90°C to 100°C, and maintain the temperature for reflux reaction for 1 hour to 2 hours; S6. Heat to 175°C to 185°C and distill for 1.5 hours at a negative pressure of ≤-0.085 MPa, removing wastewater and solvent. During the 1.5-hour distillation, precisely control the temperature fluctuation to within ±1°C and the pressure fluctuation to within ±0.005 MPa. S7. Add plant microcrystalline cellulose, stir for 1 hour, and then granulate.
2. The method for preparing a tensile-resistant plant-based cobalt salt according to claim 1, characterized in that: In step S2, arachidic acid is filtered through a filter membrane with a pore size of 0.1 μm to 0.2 μm, and the arachidic acid is preheated to 30° C. to 40° C. before being added to the reactor; Cobalt hydroxide: Detect the moisture content in cobalt hydroxide and control the moisture content below 0.5%; Plant microcrystalline cellulose: The dried plant microcrystalline cellulose is subjected to surface activation treatment, and plasma treatment technology is used to introduce active functional groups, such as hydroxyl or carboxyl groups, on its surface.
3. The method for preparing a tensile-resistant plant-based cobalt salt according to claim 1, characterized in that: In step S3, ethyl 3-ethoxypropionate is added to the reactor by dropwise addition, and the dropwise addition speed is controlled at 1 mL / min to 2 mL / min. During the dropwise addition of the solvent, stirring is performed at a stirring speed of 50 r / min to 100 r / min; Before the dropwise addition of ethyl 3-ethoxypropionate, ethyl 3-ethoxypropionate was preheated to a temperature within ±5° C. relative to the temperature in the reactor.
4. The method for preparing a tensile-resistant plant-based cobalt salt according to claim 1, characterized in that: In step S4, arachidic acid is slowly added into the reactor containing the solvent in a thin stream, and ultrasonic wave is used to assist dispersion, with the power of the ultrasonic wave set to 100W to 200W.
5. The method for preparing a tensile-resistant plant-based cobalt salt according to claim 1, characterized in that: In step S5, before adding cobalt hydroxide, cobalt hydroxide is premixed with a small amount of ethyl 3-ethoxypropionate, and then the mixture of cobalt hydroxide and ethyl 3-ethoxypropionate is added to the reactor in batches.
6. The method for preparing a tensile-resistant plant-based cobalt salt according to claim 5, characterized in that: The cobalt hydroxide and a small amount of ethyl 3-ethoxypropionate are premixed at a stirring speed of 300 r / min to 400 r / min for 5 to 10 minutes, and the mixture of cobalt hydroxide and ethyl 3-ethoxypropionate is added to the reactor in 3 to 5 batches, with an addition interval of 2 to 3 minutes for each batch.
7. The method for preparing a tensile-resistant plant-based cobalt salt according to claim 1, characterized in that: In step S6, before the distillation operation is performed, the distillation apparatus is checked for air tightness to ensure that the system is leak-free. At the same time, the distillation apparatus is preheated, and components such as the distillation flask and the condenser are preheated to 150° C. to 160° C.
8. The method for preparing a tensile-resistant plant-based cobalt salt according to claim 1, characterized in that: In step S7, when adding plant microcrystalline cellulose, it is evenly sprinkled on the surface of the reaction system and then slowly stirred. The stirring speed is initially 100 r / min to 150 r / min. As the plant microcrystalline cellulose is continuously added, the stirring speed is gradually increased to 200 r / min to 250 r / min.