CN115746343A - Black talc-based masterbatch for rubber reinforcement and preparation method thereof - Google Patents

Black talc-based masterbatch for rubber reinforcement and preparation method thereof Download PDF

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CN115746343A
CN115746343A CN202211446252.8A CN202211446252A CN115746343A CN 115746343 A CN115746343 A CN 115746343A CN 202211446252 A CN202211446252 A CN 202211446252A CN 115746343 A CN115746343 A CN 115746343A
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black talc
black
acid
rubber
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张国亮
张亚
王玲
徐泽海
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02TCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00Road transport of goods or passengers
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    • Y02T10/86Optimisation of rolling resistance, e.g. weight reduction 

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Abstract

The invention discloses a black talc-based master batch for rubber reinforcement and a preparation method thereof, wherein the black talc-based master batch comprises the following components in parts by mass: 80-100 parts of rubber matrix, 20-30 parts of modified black talcum 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 master batch for rubber reinforcement has better mechanical property and mechanical property, improves the hydrophobic effect of the black talc due to the fact that the adopted black talc is subjected to surface grafting after being activated by acid, is matched with a coupling agent for use, has uniform particle size distribution, can be effectively and uniformly dispersed in a rubber matrix, and is very suitable for the aspect of rubber reinforcement.

Description

Black talc-based masterbatch for rubber reinforcement and preparation method thereof
Technical Field
The invention relates to the technical field of rubber master batch particle preparation, in particular to a black talc-based master batch particle for rubber reinforcement and a preparation method thereof.
Background
With the rapid development of the global rubber industry, people put higher requirements on the physical and chemical properties, the processing characteristics, the product quality and other properties of raw materials in the rubber industry. In the traditional rubber manufacturing field, a large amount of powder processing aids can be used, and the problems of dust pollution and the like can be caused. Therefore, pretreatment processing of conventional rubber aids is necessary. The rubber masterbatch particles (pre-dispersed masterbatch particles) are products obtained by pre-treating traditional rubber additives which are difficult to disperse, mix or meter.
In the traditional rubber preparation process, a large amount of reinforcing filler is used as a rubber reinforcing agent, the consumption of the reinforcing filler is only second to that of rubber, the reinforcing filler is used for rubber, the strength of a rubber product can be improved, the processing performance of a rubber material can be improved, the product has various performances of good wear resistance, tear resistance, heat resistance, cold resistance, oil resistance and the like, and the service life of the product can be prolonged. The black talc is used as a novel inorganic reinforcing filler, the main mineral in the black talc is talc (containing more than 92%), the main chemical components of the black talc are silicon dioxide (containing 69%) and magnesium oxide (containing 26%), the black talc also contains a small amount of potassium, calcium, iron, sodium and other substances, in addition, the black talc also contains about 2% of organic carbon (a graphene-like layer is positioned between black talc layers), the black talc is chemically stable, has high viscosity, low hardness, certain wettability and certain amphiprotism, and compared with other traditional inorganic clay mineral materials, the black talc has more exposed siloxane structures on the surface, the hydrophobic effect is far higher than that of other inorganic clay minerals, and the dispersibility is good, so the black talc has strong application potential in the rubber product industry.
Disclosure of Invention
The invention aims to provide a preparation method of black talc-based master batch particles for rubber reinforcement.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a black talc-based masterbatch for rubber reinforcement, which comprises the following components in percentage by mass: 80-100 parts of rubber matrix, 20-30 parts of modified black talcum 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 (PEG, PEG-4000 in the embodiment of the invention) and 0.8-1 part of accelerator; the rubber matrix is one or a mixture of more than two of EPDM, SBR, NR and NBR (in one embodiment of the invention, NR is selected as the rubber matrix); the processing oil is one or a mixture of more than two of KN4006, KN4010, KN100, KN200 and KN300 (in one embodiment of the invention, KN4010 is selected);
the modified black talcum powder is prepared by the following method: (1) Soaking 1000-1500 mesh (preferably 1500 mesh) black talc raw powder into 2-4 mol/L (preferably 4 mol/L) acid aqueous solution, uniformly dispersing, stirring and refluxing for 6-12 h at 70-90 ℃ (preferably stirring and refluxing for 12h at 90 ℃), and performing after-treatment A on the obtained suspension to obtain acid-activated black talc; the acid in the acid water solution is one or a mixture of two of hydrochloric acid, sulfuric acid and nitric acid (sulfuric acid in one embodiment of the invention);
(2) Uniformly dispersing the acid activated black talc powder and methacrylic acid in the step (1) in water, carrying out stirring reflux reaction at 80-90 ℃ for 10-12 h (preferably at 90 ℃ for 12 h), and carrying out post-treatment B on the obtained reaction solution to obtain the modified black talc powder; the mass ratio of the acid activated black talc to the methacrylic acid is 1: 3-5 (preferably 1.
It is within the scope of the present invention to add other additives known in the art to the black talc based predispersed rubber masterbatch. The modified black talc of the present invention has good compatibility with several rubbers described in the present invention, and does not necessarily have similar performance improvement effects on other rubbers.
The invention also provides a black talc-based masterbatch for rubber reinforcement, which comprises the following components in mass fraction: 80-100 parts of rubber matrix, 20-30 parts of modified black talcum 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 (PEG, PEG-4000 in the embodiment of the invention) and 0.8-1 part of accelerator.
Further, the accelerator is one or a mixture of more than two of accelerator TMTD, accelerator NS, accelerator M or accelerator D, and in one embodiment of the present invention, accelerator NS.
Preferably, the coupling agent can adopt one or a mixture of more than two of phosphate coupling agent, silane coupling agent and titanate coupling agent, for example, one or a mixture of more than two of KH-560, KH-550, KH-590 and 2-hydroxyethyl methacrylate phosphate coupling agent can be adopted. In one embodiment of the present invention, a 2-hydroxyethyl methacrylate phosphate ester coupling agent is selected.
Preferably, the PEG is PEG-4000.
In one embodiment of the invention, the volume of the aqueous solution of the acid in the step (1) is 10ml/g based on the mass of the black talcum powder.
Further, the post-treatment A in the step (1) is as follows: and (3) centrifuging the suspension, washing the obtained precipitate to be neutral, drying, and crushing by using a high-speed crusher to obtain the black talc after acid activation.
In one embodiment of the present invention, the mass ratio of the acid activated black talc to the water in the step (2) is 1:30.
further, the post-treatment B in the step (1) is as follows: and centrifuging the reaction solution for 10min at 4000r/min, washing the obtained precipitate with absolute ethyl alcohol (5 times), drying (blowing and drying at 60 ℃), and crushing with a high-speed crusher to obtain the modified black talcum powder.
In a second aspect, the present invention provides a method for preparing the black talc-based masterbatch particle for rubber reinforcement, the method comprising: the modified black talc powder, the coupling agent and the polyethylene glycol are premixed, then the rubber matrix, the processing oil, the stearic acid and the accelerator are added, stirred, banburied, extruded and granulated, and the black talc-based master batch for rubber reinforcement is obtained.
Specifically, the method comprises the following steps: putting the modified black talcum powder, the coupling agent and the polyethylene glycol into an internal mixer according to the formula amount, and premixing for 10-15 min at the temperature of 60-80 ℃; and continuously adding the rubber matrix, the processing oil, the stearic acid and the accelerator according to the formula amount, stirring and banburying at the temperature of 80-100 ℃ for 25-35 min, and extruding and granulating the obtained mixture by a single-screw or double-screw extruder to obtain the black talc-based master batch for rubber reinforcement.
Further, the rotation speed of the premixing is 60-80 r/min, and the rotation speed of the stirring and banburying is 45-55 r/min.
Preferably, the screw rotating speed of the extruder is 50-60 r/min. Cutting and granulating are finished after extrusion, the average diameter of the granules is about 8-10 mm, and the average length is about 5-8 mm.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the black talc-based master batch for rubber reinforcement, the adopted black talc powder is subjected to acid activation and then surface grafting, the acid activation enables the surface of the black talc powder to have more active sites, the specific surface area of the black talc powder is increased, meanwhile, impurity removal treatment is performed on the black talc powder, and Methacrylic Acid (MA) is grafted on the surface of the acid-activated black talc powder subsequently, so that the modified black talc powder has better hydrophobicity and good lubricating effect.
2. The coupling agent and PEG are used in a matched manner, so that the synergistic promotion effect is achieved, and the dispersion effect of the modified black talc in the rubber matrix is greatly improved.
3. The superfine modified black talcum powder is added, so that the mechanical property of the rubber is greatly improved, and the viscous flow property in the mixing process can be effectively improved.
4. The black talc serving as the modified filler is prepared into the black talc-based masterbatch particles in advance, so that the subsequent application in the rubber industry is facilitated.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
The black talc raw powder in the present invention is a black talc powder which has not been chemically treated but has been mechanically treated only to have a desired particle diameter.
The 2-hydroxyethyl methacrylate phosphate ester coupling agent and PEG-4000 in the present example and the comparative example were obtained from national chemical reagent, inc., and the naphthenic oil KN4010, stearic acid, accelerator NS, etc. were obtained from domestic general chemical markets. NR is a product model ENR50 provided by santon clemine biotechnology limited.
Example 1
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 80 parts of NR rubber matrix, 20 parts of modified black talcum 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.
The preparation method of the black talc-based master batch for rubber reinforcement sequentially comprises the following steps:
1. the preparation method of the modified black talcum powder comprises the following specific preparation steps:
weighing a certain amount of 1500-mesh black talc raw powder, putting the 1500-mesh black talc raw powder into a flask, adding excessive 4mol/L sulfuric acid solution to cover the black talc powder, stirring at constant temperature for 10min to form uniform suspension, heating in a water bath at 90 ℃, stirring and refluxing for 12h, taking out the suspension, centrifuging, washing the centrifugal product with water to neutrality, drying, and crushing by using a high-speed crusher to obtain the acid activated black talc; and then uniformly stirring and mixing a certain proportion of samples (the mass ratio is acid activated black talc: methacrylic acid: water =1: 30) at room temperature, heating the mixed solution in a water bath at 90 ℃, stirring and refluxing for 12h, centrifuging for 10min at 4000r/min, washing the sediment for 5 times by using absolute ethyl alcohol, washing, blowing and drying at 60 ℃, and grinding into powder by using a high-speed grinder after drying to obtain the modified black talc.
2. According to the proportion, the modified black talc, the 2-hydroxyethyl methacrylate phosphate coupling agent and the PEG-4000 are firstly added into an internal mixer to be premixed for 10min in advance under the conditions of 70 ℃ and 70r/min of rotating speed.
3. And then adding the NR rubber matrix, the naphthenic oil KN4010, the stearic acid and the accelerator NS into the internal mixer in the step 2 in proportion, and blending and internally mixing for 35min again under the conditions of 100 ℃ and the rotating speed of 50 r/min.
4. And (3) after banburying is finished, extruding and granulating the blend obtained in the step (3) through a single-screw extruder, wherein the rotating speed of the extruder is 50r/min, the average diameter of the granules is about 8-10 mm, and the average length of the granules is about 5-8 mm, and cooling to room temperature after banburying is finished to obtain the black talc-based master batch for rubber reinforcement.
Example 2
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 90 parts of NR rubber matrix, 25 parts of modified black talcum 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 part of accelerator NS.
The preparation method and the steps of the black talc-based masterbatch for rubber reinforcement are the same as those of example 1.
Example 3
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 100 parts of NR rubber matrix, 30 parts of modified black talcum 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.
The preparation method and the steps of the black talc-based masterbatch for rubber reinforcement are the same as those of example 1.
Example 4
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 100 parts of NR rubber matrix, 20 parts of modified black talcum 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.
The preparation method and the steps of the black talc-based masterbatch for rubber reinforcement are the same as those of example 1.
Example 5
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 100 parts of NR rubber matrix, 25 parts of modified black talcum 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.
The preparation method and the steps of the black talc-based masterbatch for rubber reinforcement are the same as those of example 1.
Comparative example 1
Rubber master batch particles for non-black talc addition comprise the following components in percentage by weight: 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.
The preparation method of the rubber masterbatch without adding the black talc sequentially comprises the following steps.
1. According to the proportion, the NR rubber matrix, the 2-hydroxyethyl methacrylate phosphate coupling agent and the PEG-4000 are firstly added into an internal mixer to be premixed for 10min in advance under the conditions of 70 ℃ and 70r/min of rotation speed.
2. Then adding the naphthenic oil KN4010, the stearic acid and the accelerator NS into the internal mixer in the step 1 in proportion, and blending and internally mixing for 35min under the conditions of 100 ℃ and 50r/min of rotating speed.
3. And (3) after banburying is finished, extruding and granulating the blend obtained in the step (2) by a single-screw extruder, wherein the rotating speed of the extruder is 50r/min, the average diameter of the particles is about 8-10 mm, and the average length of the particles is about 5-8 mm, and cooling to room temperature after banburying is finished to obtain the rubber master batch without the black talc.
Comparative example 2
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 100 parts of NR rubber matrix, 20 parts of acidified black talcum 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.
The preparation method of the black talc-based masterbatch for rubber reinforcement sequentially comprises the following steps of:
1. the preparation method of the acidified black talcum powder comprises the following specific preparation steps:
weighing a certain amount of 1500-mesh black talc raw powder, putting the 1500-mesh black talc raw powder into a flask, adding excessive 4mol/L sulfuric acid solution to cover the black talc powder, stirring at constant temperature for 10min to form uniform suspension, heating in a water bath at 90 ℃, stirring and refluxing for 12h, taking out the suspension, centrifuging, washing the centrifuged product with water to neutrality, drying, and crushing with a telling crusher to obtain the acid activated black talc.
2. According to the proportion, firstly adding the black talc after acid activation, the 2-hydroxyethyl methacrylate phosphate coupling agent and the PEG-4000 into an internal mixer, and premixing the materials for 10min in advance under the conditions of 70 ℃ and 70r/min of rotating speed.
3. And then adding the NR rubber matrix, the naphthenic oil KN4010, the stearic acid and the accelerator NS into the internal mixer in the step 2 in proportion, and blending and internally mixing for 35min again under the conditions of 100 ℃ and the rotating speed of 50 r/min.
4. And (3) after banburying is finished, extruding and granulating the blend obtained in the step (3) through a single-screw extruder, wherein the rotating speed of the extruder is 50r/min, the average diameter of the granules is about 8-10 mm, and the average length of the granules is about 5-8 mm, and cooling to room temperature after banburying is finished to obtain the black talc-based master batch for rubber reinforcement.
Comparative example 3
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 100 parts of NR rubber matrix, 25 parts of acidified black talcum 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.
The above-described preparation methods and procedures of the black talc-based masterbatch pellet and the acidified black talc for rubber reinforcement were the same as those of comparative example 2.
Comparative example 4
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 100 parts of NR rubber matrix, 30 parts of acidified black talcum 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.
The above-described preparation methods and procedures of the black talc-based masterbatch pellet and the acidified black talc for rubber reinforcement were the same as those of comparative example 2.
Comparative example 5
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 100 parts of NR rubber substrate, 20 parts of surface grafted black talcum 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.
The preparation method of the black talc-based master batch for rubber reinforcement sequentially comprises the following steps:
1. the preparation method of the surface grafted black talcum powder comprises the following specific preparation steps:
uniformly mixing samples (1500-mesh black talc raw powder: methacrylic acid: water =1: 30) in a certain proportion, stirring at a constant temperature for a period of time, heating the mixed solution in a water bath at 90 ℃, stirring and refluxing for 12 hours, centrifuging for 10min at 4000r/min, washing sediments with absolute ethyl alcohol for 5 times, cleaning, blowing and drying at 60 ℃, and grinding into powder by a high-speed grinder after drying to obtain the surface-grafted black talc.
2. According to the proportion, firstly adding black talc with grafted surface, 2-hydroxyethyl methacrylate phosphate coupling agent and PEG-4000 into an internal mixer, and premixing the mixture for 10min in advance under the conditions of 70 ℃ and 70r/min of rotating speed.
3. And then adding the NR rubber matrix, naphthenic oil KN4010, stearic acid and accelerator NS into the internal mixer in the step 2 in proportion, and blending and internally mixing for 35min again under the conditions of 100 ℃ and 50r/min of rotation speed.
4. And (3) after banburying is finished, extruding and granulating the blend obtained in the step (3) through a single-screw extruder, wherein the rotating speed of the extruder is 50r/min, the average diameter of the granules is about 8-10 mm, and the average length of the granules is about 5-8 mm, and cooling to room temperature after banburying is finished to obtain the black talc-based master batch for rubber reinforcement.
Comparative example 6
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 100 parts of NR rubber substrate, 25 parts of surface grafted black talcum 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.
The above-mentioned black talc-based master batch and surface-grafted black talc for rubber reinforcement were prepared by the same procedures as in comparative example 5.
Comparative example 7
A black talc-based masterbatch for rubber reinforcement comprises the following components in parts by mass: 100 parts of NR rubber substrate, 30 parts of surface grafted black talcum 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.
The preparation methods and procedures of the black talc-based masterbatch particle and the surface grafted black talc for rubber reinforcement are the same as those of comparative example 5.
The rubber master batches prepared in the above examples and comparative examples were added to a rubber raw material to prepare a rubber product, the addition amount of the rubber master batch was 22wt.% of the rubber raw material (EPDM: SBR = 3.
TABLE 1 comparison table of mechanical properties of rubber products prepared in each example and comparative example
Figure BDA0003949675110000081
Figure BDA0003949675110000091
The invention can be better realized according to the steps. The invention can effectively improve the mechanical property and the mechanical property of the rubber product, has better compatibility with a rubber polymer matrix, and can effectively improve the processing property and the product performance of the rubber product.

Claims (10)

1. A black talc base master batch for rubber reinforcement which characterized in that: the black talc-based master batch for rubber reinforcement comprises the following components in parts by mass: 80-100 parts of rubber matrix, 20-30 parts of modified black talcum 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 more than two of EPDM, SBR, NR and NBR; the processing oil is one or a mixture of more than two of KN4006, KN4010, KN100, KN200 and KN 300;
the modified black talcum powder is prepared by the following method: (1) Soaking 1000-1500 meshes of black talc raw powder into 2-4 mol/L acid aqueous solution, uniformly dispersing, stirring and refluxing for 6-12 h at 70-90 ℃, and performing aftertreatment A on the obtained suspension to obtain acid-activated black talc; the acid in the acid water solution is one or a mixture of two of hydrochloric acid, sulfuric acid and nitric acid;
(2) Uniformly dispersing the acid activated black talc powder and methacrylic acid in the step (1) in water, stirring and refluxing at 80-90 ℃ for 10-12 h, and carrying out post-treatment B on the obtained reaction liquid to obtain the modified black talc powder; the mass ratio of the acid activated black talc to the methacrylic acid is 1:3 to 5.
2. A black talc based masterbatch for rubber reinforcement according to claim 1 wherein: the accelerator is one or a mixture of more than two of an accelerator TMTD, an accelerator NS, an accelerator M or an accelerator D.
3. A black talc based masterbatch for rubber reinforcement according to claim 1 wherein: the coupling agent is one or a mixture of more than two of phosphate coupling agent, silane coupling agent and titanate coupling agent.
4. A black talc based masterbatch for rubber reinforcement according to claim 3 wherein: the coupling agent is one or a mixture of more than two of KH-560, KH-550, KH-590 and 2-hydroxyethyl methacrylate phosphate ester coupling agents.
5. A black talc based masterbatch for rubber reinforcement according to claim 1 wherein: the processing oil is KN4010.
6. A black talc based masterbatch for rubber reinforcement according to claim 1 wherein: the polyethylene glycol is PEG-4000.
7. A black talc based masterbatch for rubber reinforcement according to claim 1 wherein: the volume of the acid water solution in the step (1) is 10ml/g based on the mass of the black talcum powder;
the post-treatment A in the step (1) is as follows: and centrifuging the suspension, washing the obtained precipitate with water to be neutral, drying and crushing to obtain the acid-activated black talc.
8. A black talc based masterbatch for rubber reinforcement according to claim 1 wherein: the mass ratio of the acid activated black talc to the water in the step (2) is 1:30;
the post-treatment B in the step (1) comprises the following steps: and centrifuging the reaction solution, washing the obtained precipitate with absolute ethyl alcohol, drying, and crushing by a high-speed crusher to obtain the modified black talcum powder.
9. A method of preparing a black talc based masterbatch for rubber reinforcement according to claim 1, characterized in that said method comprises: the modified black talcum powder, the coupling agent and the polyethylene glycol are premixed, then the rubber matrix, the processing oil, the stearic acid and the accelerator are added, and the rubber matrix, the processing oil, the stearic acid and the accelerator are stirred, mixed, extruded and granulated to obtain the black talcum-based master batch for rubber reinforcement.
10. A method of preparing black talc based masterbatch for rubber reinforcement according to claim 9 comprising: putting the modified black talcum powder, the coupling agent and the polyethylene glycol into an internal mixer according to the formula amount, and premixing for 10-15 min at the temperature of 60-80 ℃; continuously adding the rubber matrix, the processing oil, the stearic acid and the accelerator according to the formula amount, stirring and banburying at the temperature of 80-100 ℃ for 25-35 min, and extruding and granulating the obtained mixture through a single-screw or double-screw extruder to obtain the black talc-based master batch for rubber reinforcement;
the rotation speed of the premixing is 60-80 r/min, and the rotation speed of the stirring and banburying is 45-55 r/min; the rotating speed of the screw of the extruder is 50-60 r/min.
CN202211446252.8A 2022-11-18 2022-11-18 Black talc-based masterbatch for rubber reinforcement and preparation method thereof Pending CN115746343A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116284589A (en) * 2023-04-11 2023-06-23 上饶市聚微星科技有限公司 Photosensitive resin composition for additive manufacturing modified by black talc and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116284589A (en) * 2023-04-11 2023-06-23 上饶市聚微星科技有限公司 Photosensitive resin composition for additive manufacturing modified by black talc and preparation method thereof
CN116284589B (en) * 2023-04-11 2024-02-20 上饶市聚微星科技有限公司 Photosensitive resin composition for additive manufacturing modified by black talc and preparation method thereof

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