Preparation method of vulcanization-promoted cobalt salt for rubber

Abstract

The invention discloses a preparation method of vulcanization-promoted cobalt salt for rubber, and belongs to the technical field of cobalt salt preparation, the preparation method comprises the following steps: S1, preparing raw materials: 5 parts of cobalt hydroxide, 2-ethylhexoic acid, 8 parts of acetylacetone and 100 parts of water solvent; s2, raw material pretreatment: cobalt hydroxide: grinding; isocaprylic acid: carrying out preheating treatment, wherein the preheating temperature is set to be 50-60 DEG C; s3, adding water as a solvent into the reactor, slowly adding the water solvent at a constant speed, and recording the amount of added water; through the catalytic action of cobalt ions, the cross-linking reaction between rubber molecular chains is accelerated, the vulcanization time is shortened, the production efficiency is improved, meanwhile, the vulcanization reaction process is accurately controlled, a uniform and stable vulcanization network structure is obtained, and the mechanical property and durability of a rubber product are improved; the performance of vulcanized rubber is prevented from being reduced in a high-temperature or long-time use process, and the service life of a rubber product is prolonged.

Description

Technical Field

[0001] The invention belongs to the technical field of cobalt salt preparation, and in particular relates to a method for preparing a vulcanization-accelerating cobalt salt for rubber. Background Art

[0002] The rubber industry is one of the important basic industries of the national economy, and its products are widely used in tires, hoses, tapes, seals and other fields.

[0003] Vulcanization is a key step in rubber processing. It forms a cross-linked network between rubber molecular chains, thereby endowing rubber products with excellent mechanical properties, heat resistance, and aging resistance. This directly impacts the performance and service life of rubber products. However, traditional vulcanization systems rarely consider the impact on the adhesion between rubber and metal frameworks.

[0004] Traditional cobalt salts are irreplaceable in rubber with metal skeleton formulas due to their excellent adhesion-promoting function. The effect of cobalt ions requires vulcanization. Only during the vulcanization process can cobalt ions promote the cross-linking of sulfur ions in the rubber and metal ions in the skeleton, thereby enhancing the adhesion between the rubber and the metal skeleton. For this reason, we propose a method for preparing vulcanization-promoting cobalt salts for rubber. Summary of the Invention

[0005] The present invention provides a method for preparing a vulcanization-accelerating cobalt salt for rubber, so as to solve the problems raised in the above background technology.

[0006] To achieve the above object, the present invention provides the following technical solution: a method for preparing a vulcanization-accelerating cobalt salt for rubber, comprising the following steps:

[0007] S1. Raw material preparation: 5 parts of cobalt hydroxide, 1 part of 2-ethylhexanoic acid, 8 parts of acetylacetone, and 100 parts of aqueous solvent;

[0008] S2. Raw material pretreatment: cobalt hydroxide: grinding; isooctanoic acid: preheating, the preheating temperature is set to 50℃~60℃;

[0009] S3. Add water as a solvent to the reactor. When adding the water solvent, add it slowly and at a uniform rate, and record the amount of water added;

[0010] S4, add cobalt hydroxide and stir. The initial stirring speed can be set to 500r / min~600r / min. After the cobalt hydroxide is dispersed, gradually increase the stirring speed to 800r / min~900r / min. The stirring time is 30min~45min, and stirring is performed to form a pink suspension;

[0011] S5. Add acetylacetone dropwise with an interval of 3 to 5 seconds between each drop, and stir at 40°C for 2 h.

[0012] S6. Add isooctanoic acid dropwise at a rate of 2s to 3s per drop, raise the temperature to 90°C, and control the heating rate at 1°C / min to 2°C / min. Reflux for 2 hours. During the reflux reaction, install a condenser on the reflux device and use circulating condensed water to maintain the water temperature at 10°C to 15°C.

[0013] S7, the solution obtained in step S6 is centrifuged using a centrifuge tube. Before centrifugal filtration, the centrifuge tube is pre-cleaned. The centrifugal filtration time is 10 min to 15 min, and the centrifugal filtration speed is 1250 r / min;

[0014] S8, adding 100 parts of water solvent for washing and filtering, adding water solvent in portions for washing, stirring after adding water solvent, and then filtering to wash away excess impurities;

[0015] S9. Spread the product obtained in step S8 evenly on a drying plate with a thickness of 2 cm to 3 cm, and dry it at 80° C. for 8 h to obtain a finished product as a reddish-purple solid.

[0016] Furthermore, in step S1, the aqueous solvent is deionized water.

[0017] Furthermore, in step S2, the cobalt hydroxide is ground and screened through an 80-mesh sieve to screen particles with a particle size of less than 5 mm; during the preheating process of the isooctanoic acid, the temperature is continuously monitored using an accurate thermometer.

[0018] Furthermore, in step S3, a metering pump is used to add the aqueous solvent into the reactor, and the adding speed is set to 60 ml / min to 100 ml / min.

[0019] Furthermore, in step S4, the material of the blade is selected to be stainless steel or polytetrafluoroethylene, and the angle of the blade is 45°.

[0020] Furthermore, in step S5, during the dropping process, acetylacetone is dropped using a dropping device with a precision dripper and a flow rate regulating valve, and the dropping speed is set to 6ml / min to 10ml / min. During the dropping process, stirring is performed, and the stirring speed is set to 1000r / min to 1200r / min.

[0021] Furthermore, in step S6, during the dropwise addition process, isooctanoic acid is added dropwise using a dropwise addition device with a precision dripper and a flow rate regulating valve, and the dropwise addition speed is set to 6ml / min to 10ml / min. During the dropwise addition process, stirring is performed, and the stirring speed is set to 1000r / min to 1200r / min; a serpentine condenser is installed on the reflux device.

[0022] Furthermore, in step S7, before centrifugal filtration, the centrifuge tube is pre-cleaned. During the pre-cleaning process, the inside of the centrifuge tube is first thoroughly cleaned with detergent, then rinsed with a large amount of tap water, and finally rinsed with deionized water 2 to 3 times.

[0023] Furthermore, in step S8, 100 parts of aqueous solvent are added in 3 to 5 times for washing, and after the aqueous solvent is added, the mixture is stirred using a glass rod, and the stirring time can be set to 3 minutes to 5 minutes; after the stirring is completed, filter paper is used for filtration, the filter paper or filter membrane is correctly placed in the funnel, and the mixture is slowly poured to allow the filtrate to pass through the filter paper.

[0024] Furthermore, in step S9, during the drying process, thermometers are placed at different positions in the oven for monitoring.

[0025] The beneficial effects of the present invention are:

[0026] 1. The present invention accelerates the cross-linking reaction between rubber molecular chains through the catalytic effect of cobalt ions, shortens the vulcanization time, and improves production efficiency.

[0027] 2. The present invention accurately controls the vulcanization reaction process to obtain a uniform and stable vulcanization network structure, thereby improving the mechanical properties and durability of rubber products.

[0028] 3. The present invention prevents the performance of vulcanized rubber from degrading during high temperature or long-term use through the stabilizing effect of cobalt salt, thereby extending the service life of rubber products.

[0029] 4. The present invention maintains the excellent adhesion-promoting function of traditional cobalt salts in metal skeleton formulations, develops vulcanization-promoting cobalt salts suitable for different rubber types and product requirements, and expands its application in tires, hoses, tapes, seals and other fields. DETAILED DESCRIPTION

[0030] In order to further understand the content, characteristics and effects of the present invention, the following examples are listed and described in detail as follows.

[0031] Example 1:

[0032] A method for preparing a vulcanization-accelerating cobalt salt for rubber comprises the following steps:

[0033] S1. Raw material preparation: 5 parts of cobalt hydroxide, 5 parts of isooctanoic acid, 8 parts of acetylacetone, and 100 parts of aqueous solvent, wherein the aqueous solvent is deionized water;

[0034] S2. Raw material pretreatment: Grind cobalt hydroxide and screen through an 80-mesh sieve to select particles with a size of less than 5 mm; Preheat isooctanoic acid at a temperature of 50°C to 60°C, and monitor the temperature continuously using an accurate thermometer.

[0035] S3. Before adding the water solvent, make sure the inside of the reactor is clean and free of residual impurities. Then add water to the reactor as the solvent. When adding the water solvent, use a metering pump to add the water solvent to the reactor. Set the addition rate to 60 ml / min and add it slowly and evenly, while recording the amount of water added.

[0036] S4, add cobalt hydroxide and stir, the initial stirring speed can be set to 500r / min, when it is observed that the cobalt hydroxide is basically evenly dispersed, the solution becomes relatively uniform, and there is no obvious particle agglomeration, the stirring speed is gradually increased to 800r / min, the stirring time is 30min, and stirring is performed to form a pink suspension. When stirring, the blade material is selected from stainless steel or polytetrafluoroethylene, and the blade angle is 45°;

[0037] S5. Add acetylacetone dropwise. During the dropwise addition process, use a dropwise addition device with a precision dripper and a flow rate regulating valve to drop acetylacetone, and set the dropwise addition speed to 6 ml / min. The dropwise addition speed is controlled within a dropwise interval of 3 to 5 seconds. During the dropwise addition process, the stirring speed is set to 1000 r / min, and the reaction is stirred at 40° C. for 2 h.

[0038] S6, isooctanoic acid is added dropwise. During the dropwise addition process, isooctanoic acid is added dropwise using a dropping device with a precision dripper and a flow rate regulating valve, and the dropping speed is set to 6 ml / min to ensure that the isooctanoic acid added dropwise is slow and uniform. Stirring is performed during the dropwise addition process. The stirring speed is set to 1000 r / min, and the dropping speed is 2s to 3s per drop. The temperature is raised to 90°C, and the heating rate is controlled at 1°C / min. The reaction is refluxed for 2h. When the reflux reaction is carried out, a condenser is installed on the reflux device, and circulating condensed water is used to keep the water temperature at 10°C.

[0039] S7. The solution obtained in step S6 is centrifuged using a centrifuge tube. Before centrifugation, the centrifuge tube is pre-cleaned. The pre-cleaning is to thoroughly clean the inside of the centrifuge tube with detergent, then rinse with a large amount of tap water, and finally rinse with deionized water 2 to 3 times. The centrifugal filtration time is 10 min to 15 min, and the centrifugal filtration speed is 1250 r / min;

[0040] S8, adding 100 parts of water solvent for washing and filtering, when washing, adding water solvent for washing in portions, adding for washing in 3 to 5 times, and stirring after adding water solvent, using a glass rod to gently stir the mixture, the stirring time can be set to 3 minutes to 5 minutes, and then filtering, using filter paper for filtering, correctly placing the filter paper or filter membrane in the funnel, slowly pouring the mixture to allow the filtrate to pass through the filter paper to wash away excess impurities;

[0041] S9. Spread the product obtained in step S8 evenly on a drying tray. During the drying process, place thermometers at different positions in the oven for monitoring. The thickness is controlled at 2 cm to 3 cm. Dry at 80° C. for 8 h to obtain a finished product as a reddish-purple solid.

[0042] Example 2:

[0043] A method for preparing a vulcanization-accelerating cobalt salt for rubber comprises the following steps:

[0044] S1. Raw material preparation: 8 parts of cobalt hydroxide, 8 parts of isooctanoic acid, 10 parts of acetylacetone, and 125 parts of aqueous solvent, wherein the aqueous solvent is deionized water;

[0045] S2. Raw material pretreatment: Grind cobalt hydroxide and screen through an 80-mesh sieve to select particles with a size of less than 5 mm; Preheat isooctanoic acid at a temperature of 50°C to 60°C, and monitor the temperature continuously using an accurate thermometer.

[0046] S3. Before adding the water solvent, make sure the inside of the reactor is clean and free of residual impurities. Then add water to the reactor as the solvent. When adding the water solvent, use a metering pump to add the water solvent to the reactor. Set the addition rate to 70 ml / min and add it slowly and evenly, while recording the amount of water added.

[0047] S4, add cobalt hydroxide and stir, the initial stirring speed can be set to 550r / min, when it is observed that the cobalt hydroxide is basically evenly dispersed, the solution becomes relatively uniform, and there is no obvious particle agglomeration, the stirring speed is gradually increased to 850r / min, the stirring time is 40min, and stirring is performed to form a pink suspension. When stirring, the blade material is selected from stainless steel or polytetrafluoroethylene, and the blade angle is 45°;

[0048] S5. Add acetylacetone dropwise. During the dropwise addition process, use a dropwise addition device with a precision dripper and a flow rate regulating valve to drop acetylacetone, and set the dropwise addition speed to 7 ml / min. The dropwise addition speed is controlled within a dropwise interval of 3 to 5 seconds. During the dropwise addition process, the stirring speed is set to 1100 rpm, and the reaction is stirred at 40° C. for 2 h.

[0049] S6, isooctanoic acid is added dropwise. During the dropwise addition process, isooctanoic acid is added dropwise using a dropping device with a precision dripper and a flow rate regulating valve, and the dropping speed is set to 7ml / min to ensure that the isooctanoic acid added dropwise is slow and uniform. Stirring is performed during the dropwise addition process. The stirring speed is set to 1100r / min, and the dropping speed is 2s to 3s per drop. The temperature is raised to 90°C, and the heating rate is controlled at 1.5°C / min. The reaction is refluxed for 2h. When the reflux reaction is carried out, a condenser is installed on the reflux device, and circulating condensed water is used to maintain the water temperature at 13°C.

[0050] S7. The solution obtained in step S6 is centrifuged using a centrifuge tube. Before centrifugation, the centrifuge tube is pre-cleaned. The pre-cleaning is to thoroughly clean the inside of the centrifuge tube with detergent, then rinse with a large amount of tap water, and finally rinse with deionized water 2 to 3 times. The centrifugal filtration time is 10 min to 15 min, and the centrifugal filtration speed is 1250 r / min;

[0051] S8, adding 100 parts of water solvent for washing and filtering, when washing, adding water solvent for washing in portions, adding for washing in 3 to 5 times, and stirring after adding water solvent, using a glass rod to gently stir the mixture, the stirring time can be set to 3 minutes to 5 minutes, and then filtering, using filter paper for filtering, correctly placing the filter paper or filter membrane in the funnel, slowly pouring the mixture to allow the filtrate to pass through the filter paper to wash away excess impurities;

[0052] S9. Spread the product obtained in step S8 evenly on a drying tray. During the drying process, place thermometers at different positions in the oven for monitoring. The thickness is controlled at 2 cm to 3 cm. Dry at 80° C. for 8 h to obtain a finished product as a reddish-purple solid.

[0053] Example 3:

[0054] A method for preparing a vulcanization-accelerating cobalt salt for rubber comprises the following steps:

[0055] S1. Raw material preparation: 10 parts of cobalt hydroxide, 10 parts of isooctanoic acid, 12 parts of acetylacetone, and 150 parts of aqueous solvent, wherein the aqueous solvent is deionized water;

[0056] S2. Raw material pretreatment: Grind cobalt hydroxide and screen through an 80-mesh sieve to select particles with a size of less than 5 mm; Preheat isooctanoic acid at a temperature of 50°C to 60°C, and monitor the temperature continuously using an accurate thermometer.

[0057] S3. Before adding the water solvent, make sure the inside of the reactor is clean and free of residual impurities. Then add water to the reactor as the solvent. When adding the water solvent, use a metering pump to add the water solvent to the reactor. Set the addition rate to 100 ml / min and add it slowly and evenly, while recording the amount of water added.

[0058] S4, add cobalt hydroxide and stir, the initial stirring speed can be set to 600r / min, when it is observed that the cobalt hydroxide is basically evenly dispersed, the solution becomes relatively uniform, and there is no obvious particle agglomeration, the stirring speed is gradually increased to 900r / min, the stirring time is 45min, and stirring is performed to form a pink suspension. When stirring, the blade material is selected from stainless steel or polytetrafluoroethylene, and the blade angle is 45°;

[0059] S5. Add acetylacetone dropwise. During the dropwise addition process, use a dropwise addition device with a precision dripper and a flow rate regulating valve to drop acetylacetone, and set the dropwise addition speed to 10 ml / min. The dropwise addition speed is controlled within a dropwise interval of 3 to 5 seconds. During the dropwise addition process, the stirring speed is set to 1200 r / min, and the reaction is stirred at 40° C. for 2 h.

[0060] S6, isooctanoic acid is added dropwise. During the dropwise addition process, isooctanoic acid is added dropwise using a dropping device with a precision dripper and a flow rate regulating valve, and the dropping speed is set to 10 ml / min to ensure that the isooctanoic acid added dropwise is slow and uniform. Stirring is performed during the dropwise addition process. The stirring speed is set to 1200 r / min, and the dropping speed is 2s to 3s per drop. The temperature is raised to 90°C, and the heating rate is controlled at 2°C / min. The reaction is refluxed for 2h. When the reflux reaction is carried out, a condenser is installed on the reflux device, and circulating condensed water is used to keep the water temperature at 15°C.

[0061] S7. The solution obtained in step S6 is centrifuged using a centrifuge tube. Before centrifugation, the centrifuge tube is pre-cleaned. The pre-cleaning is to thoroughly clean the inside of the centrifuge tube with detergent, then rinse with a large amount of tap water, and finally rinse with deionized water 2 to 3 times. The centrifugal filtration time is 10 min to 15 min, and the centrifugal filtration speed is 1250 r / min;

[0062] S8, adding 100 parts of water solvent for washing and filtering, when washing, adding water solvent for washing in portions, adding for washing in 3 to 5 times, and stirring after adding water solvent, using a glass rod to gently stir the mixture, the stirring time can be set to 3 minutes to 5 minutes, and then filtering, using filter paper for filtering, correctly placing the filter paper or filter membrane in the funnel, slowly pouring the mixture to allow the filtrate to pass through the filter paper to wash away excess impurities;

[0063] S9. Spread the product obtained in step S8 evenly on a drying tray. During the drying process, place thermometers at different positions in the oven for monitoring. The thickness is controlled at 2 cm to 3 cm. Dry at 80° C. for 8 h to obtain a finished product as a reddish-purple solid.

[0064] From the above examples, it can be seen that under the same conditions, the present invention accelerates the cross-linking reaction between rubber molecular chains through the catalytic effect of cobalt ions, shortens the vulcanization time, and improves production efficiency.

[0065] Table 1 is a comparison of the test data of the sulfurization-accelerating cobalt salts of Examples 1 to 3 and the blank group.

[0066]

[0067] 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 vulcanization-accelerating cobalt salt for rubber, characterized in that: The following steps are involved: S1. Raw material preparation: 5 parts of cobalt hydroxide, 1 part of 2-ethylhexanoic acid, 8 parts of acetylacetone, and 100 parts of aqueous solvent; S2. Raw material pretreatment: cobalt hydroxide: grinding; isooctanoic acid: preheating, the preheating temperature is set to 50℃~60℃; S3. Add water as a solvent to the reactor. When adding the water solvent, add it slowly and at a uniform rate, and record the amount of water added; S4, add cobalt hydroxide and stir. The initial stirring speed can be set to 500r / min~600r / min. After the cobalt hydroxide is dispersed, gradually increase the stirring speed to 800r / min~900r / min. The stirring time is 30min~45min, and stirring is performed to form a pink suspension; S5, add acetylacetone dropwise, control the dropwise addition speed to 3s to 5s between each drop, and stir the reaction at 40°C for 2h; S6. Add isooctanoic acid dropwise at a rate of 2s to 3s per drop, raise the temperature to 90°C, and control the heating rate at 1°C / min to 2°C / min. Reflux for 2 hours. During the reflux reaction, install a condenser on the reflux device and use circulating condensed water to maintain the water temperature at 10°C to 15°C. S7, centrifugally filtering the solution obtained in step S6 using a centrifuge tube, the centrifugal filtration time is 10min to 15min, and the centrifugal filtration speed is 1250r / min; S8, adding 100 parts of water solvent for washing and filtering, adding water solvent in portions for washing, stirring after adding water solvent, and then filtering to wash away excess impurities; S9. Spread the product obtained in step S8 evenly on a drying plate with a thickness of 2 cm to 3 cm, and dry it at 80° C. for 8 h to obtain a finished product as a reddish-purple solid.

2. The method for preparing a vulcanization-accelerating cobalt salt for rubber according to claim 1, wherein: In step S1, deionized water is used as the aqueous solvent.

3. The method for preparing a vulcanization-accelerating cobalt salt for rubber according to claim 1, wherein: In step S2, the cobalt hydroxide is ground and screened through an 80-mesh sieve to obtain a particle size of less than 5 mm. During the preheating process of the isooctanoic acid, the temperature is continuously monitored using an accurate thermometer.

4. The method for preparing a vulcanization-accelerating cobalt salt for rubber according to claim 1, wherein: In the step S3, a metering pump is used to add the aqueous solvent into the reactor, and the adding speed is set to 60 ml / min to 100 ml / min.

5. The method for preparing a vulcanization-accelerating cobalt salt for rubber according to claim 1, wherein: In step S4, the blade material is selected from stainless steel or polytetrafluoroethylene, and the angle of the blade is 45°.

6. The method for preparing a vulcanization-accelerating cobalt salt for rubber according to claim 1, wherein: In step S5, during the dropping process, acetylacetone is dropped using a dropping device with a precision dripper and a flow rate regulating valve, and the dropping speed is set to 6ml / min to 10ml / min. During the dropping process, stirring is performed, and the stirring speed is set to 1000r / min to 1200r / min.

7. The method for preparing a vulcanization-accelerating cobalt salt for rubber according to claim 1, wherein: In step S6, during the dropwise addition process, isooctanoic acid is added dropwise using a dropwise addition device with a precision dripper and a flow rate regulating valve, and the dropwise addition speed is set to 6ml / min to 10ml / min. During the dropwise addition process, stirring is performed, and the stirring speed is set to 1000r / min to 1200r / min; a serpentine condenser is installed on the reflux device.

8. The method for preparing a vulcanization-accelerating cobalt salt for rubber according to claim 1, wherein: In step S7, before centrifugal filtration, the centrifuge tube is pre-cleaned. During the pre-cleaning process, the inside of the centrifuge tube is first thoroughly cleaned with detergent, then rinsed with a large amount of tap water, and finally rinsed with deionized water 2 to 3 times.

9. The method for preparing a vulcanization-accelerating cobalt salt for rubber according to claim 1, wherein: In step S8, 100 parts of water solvent are added in 3 to 5 times for washing, and after the water solvent is added, the mixture is stirred with a glass rod, and the stirring time can be set to 3 minutes to 5 minutes; after the stirring is completed, filter paper is used for filtering, the filter paper or filter membrane is correctly placed in the funnel, and the mixture is slowly poured to allow the filtrate to pass through the filter paper.

10. The method for preparing a vulcanization-accelerating cobalt salt for rubber according to claim 1, characterized in that: In step S9, during the drying process, thermometers are placed at different locations in the oven for monitoring.

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