A black talc-based masterbatch for rubber reinforcement and its preparation method

The modified black talc powder is prepared by acid activation and methacrylic grafting, combined with coupling agent and PEG, which solves the problems of powder additive pollution and dispersion and improves the mechanical and processing performance of rubber products.

CN115746343BActive Publication Date: 2025-08-01ZHEJIANG UNIV OF TECH
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Patent Information

Application Number
CN202211446252.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-11-18
Publication Date
2025-08-01
Estimated Expiration
2042-11-18

AI Technical Summary

Technical Problem

During the preparation of traditional rubber, powder processing aids lead to dust contamination, and the dispersion and application potential of black talc fillers in rubber are not fully utilized.

Method used

The modified black talc powder was prepared by acid activation and methacrylic grafting, combined with coupling agent and PEG, and black talc-based masterbatch was prepared to improve its dispersion and compatibility in rubber.

Benefits of technology

The dispersion effect of black talc in rubber is improved, the mechanical properties and processing properties of rubber products are improved, and the mechanical properties of rubber are enhanced.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a black talc-based masterbatch for rubber reinforcement and a preparation method thereof. By mass fraction, it comprises the following components: 80-100 parts of rubber matrix, 20-30 parts of modified black talc powder, 18-25 parts of coupling agent, 5-8 parts of processing oil, 4-6 parts of stearic acid, 2-4 parts of polyethylene glycol, and 0.8-1 part of accelerator. The black talc-based masterbatch for rubber reinforcement of the present invention has good mechanical properties and mechanical performance. Since the black talc powder used is acid-activated and then surface-grafted, the hydrophobic effect of black talc is improved. When used in combination with a coupling agent, it has a uniform particle size distribution and can be effectively and uniformly dispersed in the rubber matrix, and is very suitable for rubber reinforcement.
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Description

Technical Field

[0001] The present invention relates to the technical field of rubber masterbatch preparation, and particularly relates to a black talc-based masterbatch for rubber reinforcement and a preparation method thereof. Background Art

[0002] With the rapid development of the global rubber industry, higher requirements have been put forward for the physical and chemical properties, processing characteristics, product quality and other properties of raw materials in the rubber industry. In the traditional rubber production field, a large amount of powder processing aids are used, which will cause problems such as dust pollution. Therefore, it is necessary to preprocess and process traditional rubber aids. And rubber masterbatch (pre-dispersed masterbatch) is the product after preprocessing and processing traditional rubber aids that are difficult to disperse, mix or meter.

[0003] In the traditional rubber preparation process, a large amount of reinforcing fillers are used as rubber reinforcing agents, and their usage is second only to the rubber consumption. The reinforcing fillers used in rubber can not only improve the strength of rubber products, but also improve the processing performance of rubber compounds, and endow the products with various properties such as good abrasion resistance, tear resistance, heat resistance, cold resistance, and oil resistance, and can extend the service life of the products. And black talc, as a new type of inorganic reinforcing filler, the main mineral in black talc is talc (containing more than 92%), its main chemical components are silicon dioxide (about 69%) and magnesium oxide (about 26%), and it also contains a small amount of potassium, calcium, iron, sodium and other substances. In addition, it also contains about 2% of organic carbonaceous matter (graphene-like layers are located between the black talc layers). Black talc is chemically stable, has high viscosity, low hardness, has a certain wettability and also has a certain amphoteric property. And compared with other traditional inorganic clay mineral materials, its surface has more exposed siloxane structures, and the hydrophobic effect is much higher than that of other inorganic clay minerals, and the dispersibility is good. Therefore, black talc has great application potential in the rubber product industry. Summary of the Invention

[0004] The purpose of the present invention is to provide a preparation method of a black talc-based masterbatch for rubber reinforcement. The black talc-based masterbatch for rubber reinforcement prepared by the present invention can not only effectively improve the mechanical and mechanical properties of the rubber masterbatch, but also effectively improve the dispersion effect of the black talc filler in the rubber, and is very suitable for the reinforcement of rubber products.

[0005] To achieve this purpose, the present invention adopts the following technical solutions:

[0006] In a first aspect, the present invention provides a black talc-based masterbatch for rubber reinforcement, which, by mass fraction, comprises the following components: 80 to 100 parts of a rubber matrix, 20 to 30 parts of modified black talc powder, 18 to 25 parts of a coupling agent, 5 to 8 parts of a processing oil, 4 to 6 parts of stearic acid, 2 to 4 parts of polyethylene glycol (PEG, PEG-4000 in the examples of the present invention), and 0.8 to 1 part of an accelerator; the rubber matrix is one or a mixture of two or more of EPDM, SBR, NR, and NBR (NR is selected as the rubber matrix in one embodiment of the present invention); the processing oil is one or a mixture of two or more of KN4006, KN4010, KN100, KN200, and KN300 (KN4010 is selected in one embodiment of the present invention).

[0007] The modified black talc powder is prepared by the following method: (1) Immerse black talc raw powder with a mesh size of 1000 to 1500 (preferably 1500 mesh) in an aqueous solution of an acid with a concentration of 2 to 4 mol / L (preferably 4 mol / L), stir and reflux at 70 to 90 °C for 6 to 12 h (preferably stir and reflux at 90 °C for 12 h) after uniform dispersion, and the obtained suspension is subjected to post-treatment A to obtain acid-activated black talc; the acid in the aqueous solution of the acid is one or a mixture of two of hydrochloric acid, sulfuric acid, and nitric acid (sulfuric acid in one embodiment of the present invention).

[0008] (2) Uniformly disperse the acid-activated black talc and methacrylic acid in step (1) in water, stir and reflux at 80 to 90 °C for 10 to 12 h (preferably stir and reflux at 90 °C for 12 h), and the obtained reaction solution is subjected to post-treatment B to obtain the modified black talc powder; the mass ratio of the acid-activated black talc to methacrylic acid is 1:3 to 5 (preferably 1:5, and when the dosage of methacrylic acid continues to increase, the performance does not improve significantly).

[0009] Adding other additives well-known in the art to the black talc-based pre-dispersed rubber masterbatch should also be within the protection scope of the present invention. The modified black talc of the present invention has good compatibility with several rubbers described in the present invention, and similar performance improvement effects may not occur for other rubbers.

[0010] The present invention also provides a black talc-based masterbatch for rubber reinforcement, which, by mass fraction, consists of the following components: 80 to 100 parts of a rubber matrix, 20 to 30 parts of modified black talc powder, 18 to 25 parts of a coupling agent, 5 to 8 parts of a processing oil, 4 to 6 parts of stearic acid, 2 to 4 parts of polyethylene glycol (PEG, PEG-4000 in the examples of the present invention), and 0.8 to 1 part of an accelerator.

[0011] Further, the accelerator is one or a mixture of two or more of accelerator TMTD, accelerator NS, accelerator M, or accelerator D, and is accelerator NS in an embodiment of the present invention.

[0012] Preferably, the coupling agent can be one or a mixture of two or more of phosphate ester coupling agents, silane coupling agents, and titanate coupling agents, such as one or a mixture of two or more of KH-560, KH-550, KH-590, and 2-hydroxyethyl methacrylate phosphate coupling agent. 2-hydroxyethyl methacrylate phosphate coupling agent is selected in an embodiment of the present invention.

[0013] Preferably, the PEG is PEG-4000.

[0014] In an embodiment of the present invention, the volume of the aqueous solution of the acid in step (1) is 10 ml / g based on the mass of the black talc powder.

[0015] Further, the post-treatment A in step (1) is: centrifuging the suspension, washing the obtained precipitate with water until neutral, drying, and (using a high-speed pulverizer) pulverizing to obtain the acid-activated black talc.

[0016] In an embodiment of the present invention, the mass ratio of the acid-activated black talc to the water in step (2) is 1:30.

[0017] Further, the post-treatment B in step (1) is: centrifuging the reaction solution (centrifuging at 4000 r / min for 10 min), washing the obtained precipitate with absolute ethanol (5 times), drying (drying by blowing air at 60 °C), and pulverizing with a high-speed pulverizer to obtain the modified black talc powder.

[0018] In a second aspect, the present invention provides a method for preparing the above-mentioned black talc-based masterbatch for rubber reinforcement, and the method is: premixing the formulated amount of modified black talc powder, coupling agent, and polyethylene glycol, then adding the formulated amount of rubber matrix, processing oil, stearic acid, and accelerator, stirring and kneading, and extruding and pelletizing to obtain the black talc-based masterbatch for rubber reinforcement.

[0019] Specifically, the method is: putting the formulated amount of modified black talc powder, coupling agent, and polyethylene glycol into a kneader, premixing at 60-80 °C for 10-15 min; then continuously adding the formulated amount of rubber matrix, processing oil, stearic acid, and accelerator, stirring and kneading at 80-100 °C for 25-35 min, and extruding and pelletizing the obtained mixture through a single-screw or twin-screw extruder to obtain the black talc-based masterbatch for rubber reinforcement.

[0020] Further, the rotation speed of the premixing is 60 - 80 r / min, and the rotation speed of the stirring and kneading is 45 - 55 r / min.

[0021] Preferably, the screw rotation speed of the extruder is 50 - 60 r / min. After extrusion, cutting and granulation are completed, and the average diameter of the particles is about 8 - 10 mm, and the average length is about 5 - 8 mm.

[0022] The present invention has the following beneficial effects compared with the prior art:

[0023] 1. For the black talc-based masterbatch for rubber reinforcement of the present invention, since the black talc powder used is surface grafted after acid activation, the acid activation makes the surface of the black talc have more active sites, which not only increases the specific surface area of the black talc but also removes impurities from the black talc. Subsequently, methyl methacrylate (MA) is grafted on the surface of the acid-activated black talc, which can make the modified black talc powder have better hydrophobicity and good lubrication effect.

[0024] 2. The use of a coupling agent and PEG in combination has a synergistic promoting effect, greatly improving the dispersion effect of the modified black talc in the rubber matrix.

[0025] 3. The addition of ultra-fine modified black talc powder greatly improves the mechanical properties of the rubber and can effectively improve the viscous flow property during the mixing process.

[0026] 4. The black talc as a modified filler is pre-prepared into a black talc-based masterbatch, which is convenient for subsequent application in the rubber industry. Specific Embodiments

[0027] The following describes the preferred embodiments of the present invention. It should be understood that the preferred embodiments described herein are only for the purpose of illustrating and explaining the present invention, and are not used to limit the present invention.

[0028] The black talc raw powder in the present invention refers to black talc powder that has not been chemically treated and has only been mechanically treated to the required particle size.

[0029] In this embodiment and the comparative example, the 2-hydroxyethyl methacrylate phosphate coupling agent and PEG-4000 are purchased from Sinopharm Chemical Reagent Co., Ltd., and the naphthenic oil KN4010, stearic acid, accelerator NS, etc. are all purchased from the domestic general chemical market. The NR is a product with the model ENR50 provided by Shandong Klein Biotechnology Co., Ltd.

[0030] Example 1

[0031] A black talc-based masterbatch for rubber reinforcement, by mass, comprises the following components: 80 parts of NR rubber matrix, 20 parts of modified black talc powder, 18 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 5 parts of naphthenic oil KN4010, 4 parts of stearic acid, 2 parts of polyethylene glycol (PEG-4000), and 0.8 part of accelerator NS.

[0032] The preparation method of the above black talc-based masterbatch for rubber reinforcement successively comprises the following steps:

[0033] 1. Preparation of modified black talc powder, and its specific preparation steps are as follows:

[0034] Weigh a certain amount of 1500-mesh raw black talc powder and place it in a flask. Add an excessive amount of 4 mol / L sulfuric acid solution to submerge the black talc powder. The volume of the sulfuric acid solution is 10 ml / g based on the mass of the black talc powder. Stir at a constant temperature for 10 min to form a uniform suspension. Then, stir and reflux in a 90°C water bath for 12 h. Finally, take out the suspension for centrifugation. After washing the centrifuged product with water until neutral and drying it, crush it with a high-speed pulverizer to obtain acid-activated black talc. Then, mix a certain proportion of samples (mass ratio of acid-activated black talc: methacrylic acid: water = 1:5:30) evenly by stirring at room temperature. Then, heat the mixed solution in a 90°C water bath, stir and reflux for 12 h, and then centrifuge at 4000 r / min for 10 min. Wash the sediment with anhydrous ethanol 5 times. After washing, dry it in a blast dryer at 60°C. After drying, grind it into powder with a high-speed pulverizer to obtain the modified black talc.

[0035] 2. According to the above proportion, first add the modified black talc, 2-hydroxyethyl methacrylate phosphate coupling agent, and PEG-4000 to a mixer and premix them for 10 min at 70°C and a rotation speed of 70 r / min.

[0036] 3. Then, put the NR rubber matrix, naphthenic oil KN4010, stearic acid, and accelerator NS into the mixer in step 2 according to the proportion, and remix and knead them again for 35 min at 100°C and a rotation speed of 50 r / min.

[0037] 4. After kneading is completed, extrude and pelletize the blend in step 3 through a single-screw extruder. The rotation speed of the extruder is 50 r / min. The average diameter of the pellets is about 8 - 10 mm, and the average length is about 5 - 8 mm. After that, cool it to room temperature to obtain the above black talc-based masterbatch for rubber reinforcement.

[0038] Example 2

[0039] A black talc-based masterbatch for rubber reinforcement comprises the following components, calculated by weight: 90 parts of NR rubber matrix, 25 parts of modified black talc powder, 22 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 6 parts of naphthenic oil KN4010, 5 parts of stearic acid, 3 parts of polyethylene glycol (PEG-4000), and 0.9 parts of accelerator NS.

[0040] The preparation method and steps of the black talc-based masterbatch for rubber reinforcement are the same as those in Example 1.

[0041] Example 3

[0042] A black talc-based masterbatch for rubber reinforcement comprises the following components, calculated by weight: 100 parts of NR rubber matrix, 30 parts of modified black talc powder, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0043] The preparation method and steps of the black talc-based masterbatch for rubber reinforcement are the same as those in Example 1.

[0044] Example 4

[0045] A black talc-based masterbatch for rubber reinforcement comprises the following components, calculated by weight: 100 parts of NR rubber matrix, 20 parts of modified black talc powder, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0046] The preparation method and steps of the black talc-based masterbatch for rubber reinforcement are the same as those in Example 1.

[0047] Example 5

[0048] A black talc-based masterbatch for rubber reinforcement comprises the following components, calculated by weight: 100 parts of NR rubber matrix, 25 parts of modified black talc powder, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0049] The preparation method and steps of the black talc-based masterbatch for rubber reinforcement are the same as those in Example 1.

[0050] Comparative Example 1

[0051] A rubber masterbatch without black talc, by weight percentage, comprises the following components: 100 parts of NR rubber matrix, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0052] The preparation method of the above rubber masterbatch without black talc successively comprises the following steps.

[0053] 1. According to the stated ratio, first add the NR rubber matrix, 2-hydroxyethyl methacrylate phosphate coupling agent, and PEG-4000 into a kneader, and premix them in advance for 10 min at 70 °C and a rotation speed of 70 r / min.

[0054] 2. Then put the naphthenic oil KN4010, stearic acid, and accelerator NS into the kneader in step 1 according to the ratio, and co-knead and mix them again for 35 min at 100 °C and a rotation speed of 50 r / min.

[0055] 3. After the kneading is completed, extrude and pelletize the blend in step 2 through a single-screw extruder. The rotation speed of the extruder is 50 r / min. The average diameter of the pellets is about 8 - 10 mm, and the average length is about 5 - 8 mm. After that, cool it to room temperature to obtain the rubber masterbatch without black talc.

[0056] Comparative Example 2

[0057] A black talc-based masterbatch for rubber reinforcement, by mass parts, comprises the following components: 100 parts of NR rubber matrix, 20 parts of acidified black talc powder, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0058] The preparation method of the above black talc-based masterbatch for rubber reinforcement successively comprises the following steps:

[0059] 1. Preparation of acidified black talc powder, and its specific preparation steps are as follows:

[0060] Weigh a certain amount of 1500-mesh black talc raw powder and put it into a flask. Add an excessive amount of 4 mol / L sulfuric acid solution to submerge the black talc powder. The volume of the sulfuric acid solution is 10 ml / g based on the mass of the black talc powder. Stir it at a constant temperature for 10 min to form a uniform suspension. Then stir and reflux it in a 90 °C water bath for 12 h. Finally, take out the suspension and centrifuge it. Wash the centrifuged product with water until it is neutral and then dry it. Crush it with a high-speed grinder to obtain acid-activated black talc.

[0061] 2. According to the above ratio, acid-activated black talc, 2-hydroxyethyl methacrylate phosphate coupling agent, and PEG-4000 were first added to an internal mixer and pre-mixed at 70° C. and 70 r / min for 10 minutes.

[0062] 3. The NR rubber matrix, naphthenic oil KN4010, stearic acid, and accelerator NS were added to the internal mixer of step 2 in proportion, and mixed and kneaded again at 100° C. and a rotation speed of 50 r / min for 35 min.

[0063] 4. After the mixing is completed, the blend in step 3 is extruded into granules through a single-screw extruder at a speed of 50 r / min. The average diameter of the granules is about 8 to 10 mm and the average length is about 5 to 8 mm. After cooling to room temperature, the black talc-based masterbatch for rubber reinforcement can be obtained.

[0064] Comparative Example 3

[0065] A black talc-based masterbatch for rubber reinforcement comprises the following components, calculated by weight: 100 parts of NR rubber matrix, 25 parts of acidified black talc powder, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0066] The preparation methods and steps of the black talc-based masterbatch and acidified black talc for rubber reinforcement are the same as those in Comparative Example 2.

[0067] Comparative Example 4

[0068] A black talc-based masterbatch for rubber reinforcement comprises the following components, calculated by weight: 100 parts of NR rubber matrix, 30 parts of acidified black talc powder, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0069] The preparation methods and steps of the black talc-based masterbatch and acidified black talc for rubber reinforcement are the same as those in Comparative Example 2.

[0070] Comparative Example 5

[0071] A black talc-based masterbatch for rubber reinforcement comprises the following components, calculated by weight: 100 parts of NR rubber matrix, 20 parts of surface-grafted black talc powder, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0072] The preparation method of the above-mentioned black talc-based masterbatch for rubber reinforcement successively includes the following steps:

[0073] 1. Preparation of surface-grafted black talc powder, and its specific preparation steps are as follows:

[0074] Mix a certain proportion of samples (mass ratio: 1500-mesh black talc raw powder: methacrylic acid: water = 1:5:30) evenly, stir at a constant temperature for a period of time, then heat and stir the mixture under reflux in a water bath at 90°C for 12 hours, then centrifuge at 4000 r / min for 10 minutes, wash the sediment with anhydrous ethanol 5 times, and after washing, dry it in a blast dryer at 60°C. After drying, grind it into powder with a high-speed grinder to obtain the surface-grafted black talc.

[0075] 2. According to the above-mentioned proportion, first add the surface-grafted black talc, 2-hydroxyethyl methacrylate phosphate coupling agent, and PEG-4000 to the internal mixer, and premix them for 10 minutes at 70°C and a rotation speed of 70 r / min.

[0076] 3. Then put the NR rubber matrix, naphthenic oil KN4010, stearic acid, and accelerator NS into the internal mixer in step 2 according to the proportion, and remix and knead them again for 35 minutes at 100°C and a rotation speed of 50 r / min.

[0077] 4. After kneading is completed, extrude and pelletize the blend in step 3 through a single-screw extruder. The rotation speed of the extruder is 50 r / min, the average diameter of the pellets is about 8 - 10 mm, and the average length is about 5 - 8 mm. After that, cool it to room temperature to obtain the black talc-based masterbatch for rubber reinforcement.

[0078] Comparative Example 6

[0079] A black talc-based masterbatch for rubber reinforcement, in parts by mass, includes the following components: 100 parts of NR rubber matrix, 25 parts of surface-grafted black talc powder, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0080] The preparation method and steps of the above-mentioned black talc-based masterbatch for rubber reinforcement and surface-grafted black talc are the same as those in Comparative Example 5.

[0081] Comparative Example 7

[0082] A black talc-based masterbatch for rubber reinforcement, by mass parts, comprises the following components: 100 parts of NR rubber matrix, 30 parts of surface-grafted black talc powder, 25 parts of 2-hydroxyethyl methacrylate phosphate coupling agent, 8 parts of naphthenic oil KN4010, 6 parts of stearic acid, 4 parts of polyethylene glycol (PEG-4000), and 1 part of accelerator NS.

[0083] The above-mentioned black talc-based masterbatch for rubber reinforcement and the preparation method and steps of the surface-grafted black talc are the same as those in Comparative Example 5.

[0084] The rubber masterbatch prepared in each of the above examples and comparative examples was added to the rubber raw material to prepare a rubber product. The addition amount of the rubber masterbatch was 22 wt.% of the rubber raw material (EPDM:SBR = 3:1), and the mechanical properties were tested. The preparation of the mechanical property test specimens was all carried out with reference to the national standard HG / T 3868-2008. The test results of the rubber products are shown in Table 1.

[0085] Table 1 Comparison table of mechanical properties of rubber products made in each example and comparative example

[0086]

[0087]

[0088] According to the above steps, the present invention can be preferably realized. The present invention can effectively improve the mechanical properties and mechanical performance of rubber products, and has better compatibility with the rubber polymer matrix, and can effectively improve the processing performance and product performance of rubber products.

Claims

1. A black talc-based masterbatch for rubber reinforcement, characterized in that: The black talc-based masterbatch for rubber reinforcement comprises the following components by mass fraction: 80-100 parts of rubber matrix, 20-30 parts of modified black talc powder, 18-25 parts of coupling agent, 5-8 parts of processing oil, 4-6 parts of stearic acid, 2-4 parts of polyethylene glycol, and 0.8-1 part of accelerator; the rubber matrix is one or a mixture of two or more of EPDM, SBR, NR, and NBR; the processing oil is one or a mixture of two or more of KN4006, KN4010, KN100, KN200, and KN300; The modified black talc powder is prepared by the following method: (1) Immerse the 1000-1500 mesh black talc raw powder in an aqueous solution of an acid with a concentration of 2-4 mol / L, uniformly disperse it, and stir and reflux at 70-90 °C for 6-12 h. The obtained suspension is subjected to post-treatment A to obtain acid-activated black talc; the acid in the aqueous solution of the acid is one or a mixture of two of hydrochloric acid, sulfuric acid, and nitric acid; (2) Uniformly disperse the acid-activated black talc and methacrylic acid in step (1) in water, stir and reflux at 80-90 °C for 10-12 h, and subject the obtained reaction solution to post-treatment B to obtain the modified black talc powder; the mass ratio of the acid-activated black talc to methacrylic acid is 1:3-5.

2. The black talc-based masterbatch for rubber reinforcement according to claim 1, wherein: The accelerator is one or a mixture of two or more of accelerator TMTD, accelerator NS, accelerator M, and accelerator D.

3. The black talc-based masterbatch for rubber reinforcement according to claim 1, characterized in that: The coupling agent is one or a mixture of two or more of phosphate ester coupling agent, silane coupling agent, and titanate coupling agent.

4. The black talc-based masterbatch for rubber reinforcement according to claim 3, wherein: The coupling agent is one or a mixture of two or more of KH-560, KH-550, KH-590, and 2-hydroxyethyl methacrylate phosphate coupling agent.

5. The black talc-based masterbatch for rubber reinforcement according to claim 1, characterized in that: The processing oil is KN4010.

6. The black talc-based masterbatch for rubber reinforcement according to claim 1, wherein: The polyethylene glycol is PEG-4000.

7. The black talc-based masterbatch for rubber reinforcement according to claim 1, characterized in that: In step (1), the volume of the aqueous solution of the acid is 10 ml / g based on the mass of the black talc powder. The post-treatment A in step (1) is: centrifuge the suspension, wash the obtained precipitate with water until neutral, dry it, and pulverize it to obtain the acid-activated black talc.

8. The black talc-based masterbatch for rubber reinforcement according to claim 1, wherein: In step (2), the mass ratio of the acid-activated black talc to the water is 1:

30. The post-treatment B in step (1) is: centrifuge the reaction solution, wash the obtained precipitate with absolute ethanol, dry it, and pulverize it with a high-speed pulverizer to obtain the modified black talc powder.

9. The preparation method of the black talc-based masterbatch for rubber reinforcement according to claim 1, characterized in that The method is: premix the formulated amount of modified black talc powder, coupling agent, and polyethylene glycol, then add the formulated amount of rubber matrix, processing oil, stearic acid, and accelerator, stir and knead, and extrude and granulate to obtain the black talc-based masterbatch for rubber reinforcement.

10. The preparation method of the black talc-based masterbatch for rubber reinforcement according to claim 9, characterized in that The method is: put the formulated amount of modified black talc powder, coupling agent, and polyethylene glycol into a kneader, premix at 60-80 °C for 10-15 min; continue to add the formulated amount of rubber matrix, processing oil, stearic acid, and accelerator, stir and knead at 80-100 °C for 25-35 min, and extrude and granulate the obtained mixture through a single-screw or twin-screw extruder to obtain the black talc-based masterbatch for rubber reinforcement; The rotation speed of the premixing is 60 - 80 r / min, the rotation speed of the stirring and kneading is 45 - 55 r / min; the screw rotation speed of the extruder is 50 - 60 r / min.

Citation Information

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