CN113528055A - Environment-friendly all-steel transition layer adhesive and preparation method thereof - Google Patents
Environment-friendly all-steel transition layer adhesive and preparation method thereof Download PDFInfo
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- CN113528055A CN113528055A CN202110794042.7A CN202110794042A CN113528055A CN 113528055 A CN113528055 A CN 113528055A CN 202110794042 A CN202110794042 A CN 202110794042A CN 113528055 A CN113528055 A CN 113528055A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J107/00—Adhesives based on natural rubber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
- B29B7/005—Methods for mixing in batches
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention belongs to the technical field of rubber, and particularly relates to environment-friendly all-steel transition layer rubber and a preparation method thereof. The environment-friendly all-steel transition layer adhesive comprises the following components in parts by weight: 100 parts of natural rubber, 50-60 parts of carbon black, 0.1-3 parts of carbon nano tubes, 3-8 parts of zinc oxide, 1-4 parts of tackifying resin, 0.5-2 parts of modified methyl resin, 1-3 parts of anti-aging agent, 0.2-1 part of cobalt salt, 652-6 parts of adhesive, 0.5-2 parts of accelerator DZ, 3-7 parts of insoluble sulfur powder and 0.1-0.5 part of anti-scorching agent CTP. According to the environment-friendly all-steel transition layer adhesive, resorcinol is replaced by the modified resorcinol methyl 396, and due to the fact that the mass fraction of free resorcinol in the modified resorcinol methyl is extremely low, little smoke generated by sublimation of the free resorcinol can be avoided in the processing process of the adhesive material, environmental pollution is reduced, and the environment-friendly all-steel transition layer adhesive is beneficial to the health of staff; meanwhile, the prepared rubber material has better adhesive force, low heat generation and excellent tear resistance, and can further prolong the service life of the tire.
Description
Technical Field
The invention belongs to the technical field of rubber, and particularly relates to environment-friendly all-steel transition layer rubber and a preparation method thereof.
Background
Since the European Union implements the tire labeling method, the tire industry in China is urgently required to be upgraded in green under the situation. The green tire is an energy-saving, environment-friendly and safe tire product, the whole production process is in a green manufacturing concept, and the application process advocates green use. The transition layer rubber of the belt speed layer, the tire body and the inner liner of the all-steel radial tire needs to have better adhesive property with the steel wire cord, at present, the steel wire adhesive system of the rubber materials in China generally adopts a m-A-white-cobalt system or a m-A-cobalt system, and because the pure resorcinol used in the adhesive system has lower relative molecular mass, the rubber materials can be sublimated to generate smoke in the processing process, so the environment is seriously polluted, and the health of staff is harmed. With the stricter and stricter national environmental protection policies, enterprises face the environmental protection pressure of the production process, so that the domestic tire enterprises actively explore how to make the tire production and manufacturing process more environment-friendly.
Disclosure of Invention
The invention aims to overcome and supplement the defects in the prior art, and provides the environment-friendly all-steel transition layer adhesive, which can ensure that the production process of the all-steel transition layer adhesive is more environment-friendly, improve the adhesive force, low heat generation and tear resistance of the all-steel transition layer adhesive, and further prolong the service life of a tire. The environment-friendly all-steel transition layer adhesive disclosed by the invention almost has no free resorcinol volatile component in the production process, and can effectively solve the problem of environmental pollution caused by resorcinol volatilization in the processing process; simultaneously has better adhesive force, low heat generation and excellent tear resistance, and can further prolong the service life of the tire through the improvement.
In a first aspect, the embodiment of the invention provides an environment-friendly all-steel transition layer adhesive, which comprises the following components in parts by weight: 100 parts of natural rubber, 50-60 parts of carbon black, 0.1-3 parts of carbon nano tubes, 3-8 parts of zinc oxide, 1-4 parts of tackifying resin, 0.5-2 parts of modified methyl methacrylate resin, 1-3 parts of anti-aging agent, 0.2-1 part of cobalt salt, 652-6 parts of adhesive, 0.5-2 parts of accelerator DZ, 3-7 parts of insoluble sulfur powder and 0.1-0.5 part of anti-scorching agent CTP.
Further, the carbon black is one or both of N330 and N326.
Further, the carbon nano tube is a gas phase precipitation method multi-wall agglomeration type carbon nano tube, the tube diameter is 12-15 nm, the length is 3-10 mu m, and the specific surface area is 250-290 m2/g。
Further, the modified m-methyl resin is formed by polymerization reaction of resorcinol, dicyclopentadiene and formaldehyde, and specifically comprises at least one compound represented by formula (I), formula (II) and formula (III), and the chemical formula is as follows:
in the formulae (I), (II) and (III), n is a natural number other than 0, and R is-CH (CH)3)C5H5Or H.
Further, the cobalt salt is cobalt boroacylate or cobalt neodecanoate.
Further, the tackifying resin is one or two of C5 tackifying resin, 203 tackifying resin and 204 tackifying resin.
Further, the anti-aging agent is two or three of an anti-aging agent 4020, an anti-aging agent RD and an anti-aging agent 3100.
Further, the insoluble sulfur IS insoluble sulfur OT-20 or insoluble sulfur IS 6033.
In a second aspect, an embodiment of the present invention provides a preparation method of the environment-friendly all-steel transition layer rubber, which adopts a one-step continuous low-temperature mixing (OMS low-temperature mixing) process, and includes the following steps:
(1) mixing master batch by an internal mixer: putting 100 parts of natural rubber, 50-60 parts of carbon black, 0.1-3 parts of carbon nano tubes, 3-8 parts of zinc oxide, 1-4 parts of tackifying resin, 0.5-2 parts of modified methyl resin, 1-3 parts of anti-aging agent and 0.2-1 part of cobalt salt into an internal mixer for mixing, wherein the upper top plug pressure is 6-18 MPa, the rotor speed is 40-50 r/min, the rubber discharge temperature is 140-155 ℃, and the time is 135-160 s, so as to obtain masterbatch;
(2) mixing the final rubber mixing with an open mill: directly conveying the masterbatch obtained in the step (1) to an open mill for supplementary mixing and cooling, when the temperature of the masterbatch is less than or equal to 75 ℃, putting 2-6 parts of an adhesive RA65, 0.5-2 parts of an accelerant DZ, 3-7 parts of insoluble sulfur powder and 0.1-0.5 part of an anti-coking agent CTP into the open mill for mixing, controlling the roll spacing of the open mill to be 2.5-4 mm, controlling the rotating speed of the open mill to be 20-40 r/min, controlling the rubber discharge temperature to be 85-100 ℃, controlling the mixing time of the open mill to be 600-800 seconds, and obtaining the environment-friendly all-steel transition layer rubber after mixing.
Further, a GK320E internal mixer is adopted in the internal mixer in the step (1), and a phi 660X 2130mm open mill is adopted in the open mill in the step (2).
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
(1) according to the environment-friendly all-steel transition layer adhesive, resorcinol is replaced by the novel modified resorcinol methyl 396, and due to the fact that the mass fraction of free resorcinol in the modified resorcinol methyl 396 is extremely low, the situation that smoke is generated due to sublimation of the free resorcinol in the processing process of an adhesive material is little, environmental pollution is reduced, and staff health is facilitated; (2) the addition of the carbon nano tube can improve the tear resistance of the transition layer adhesive and reduce heat generation; (3) the carbon nano tube and the modified meta-resin have synergistic effect to improve the adhesive force of the aged transition layer adhesive; (4) the novel modified meta-resin can meet the use requirement of the all-steel transition layer rubber performance, so that a new development direction can be explored for the tire rubber formula summation and the production and manufacturing process which are more environment-friendly.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The environment-friendly all-steel transition layer adhesive comprises the following components in parts by weight: 100 parts of natural rubber, 53 parts of carbon black N326, 1 part of carbon nanotube GT-300, 7 parts of zinc oxide, 2 parts of 204 tackifying resin, 1.5 parts of modified methyl methacrylate resin 396, 2 parts of anti-aging agent 4020, 1 part of anti-aging agent RD, 0.4 part of cobalt boroacylate, 5 parts of adhesive RA65, 1.3 parts of accelerator DZ, 4.2 parts of insoluble sulfur powder OT-20 and 0.2 part of anti-scorching agent CTP.
A preparation method of environment-friendly all-steel transition layer rubber adopts a one-step continuous low-temperature mixing (OMS low-temperature mixing) process, and comprises the following steps:
mixing master batch by an internal mixer: putting natural rubber, carbon black N326, carbon nano tube DT-300, zinc oxide, tackifying resin 204, modified meta-methyl resin 396, anti-aging agent 4020 and cobalt boroacylate into an internal mixer for mixing, wherein the upper plug pressure is 18MPa, the rotor speed is 45r/min, the rubber discharge temperature is 150 ℃, and the time is 140s, so as to obtain a master batch;
mixing the final rubber mixing with an open mill: and (2) directly conveying the master batch obtained in the step (1) to an open mill for supplementary mixing and cooling, when the temperature of the glue is less than or equal to 75 ℃, putting an adhesive RA65, an accelerant DZ, insoluble sulfur powder OT-20 and an anti-scorching agent CTP into the open mill for mixing, wherein the roll spacing of the open mill is set to be 3mm, the rotating speed of the open mill is set to be 30r/min, the glue discharging temperature is set to be 95 ℃, and the mixing time of the open mill is set to be 700 seconds, so that the environment-friendly all-steel transition layer glue is obtained.
Example 2
The environment-friendly all-steel transition layer adhesive comprises the following components in parts by weight: 100 parts of natural rubber, 53 parts of carbon black N326, 1.5 parts of carbon nanotube GT-300, 7 parts of zinc oxide, 2 parts of 204 tackifying resin, 1.5 parts of modified methyl methacrylate resin 396, 2 parts of anti-aging agent 4020, 1 part of anti-aging agent RD, 0.4 part of cobalt boroacylate, 5 parts of adhesive RA65, 1.3 parts of accelerator DZ, 4.2 parts of insoluble sulfur powder OT-20 and 0.2 part of scorch retarder CTP.
A preparation method of environment-friendly all-steel transition layer rubber adopts a one-step continuous low-temperature mixing (OMS low-temperature mixing) process, and comprises the following steps:
mixing master batch by an internal mixer: putting natural rubber, carbon black N326, carbon nano tube DT-300, zinc oxide, 204 tackifying resin, modified meta-methyl resin 396, an anti-aging agent RD and cobalt boroacylate into an internal mixer for mixing, wherein the top plug pressure is 18MPa, the rotor speed is 45r/min, the rubber discharge temperature is 150 ℃, and the time is 140s, so as to obtain master batch;
mixing the final rubber mixing with an open mill: and (2) directly conveying the master batch obtained in the step (1) to an open mill for supplementary mixing and cooling, when the glue temperature is less than or equal to 75 ℃, putting the adhesive RA65, the accelerant DZ, the insoluble sulfur powder and the anti-coking agent into the open mill for mixing, wherein the roll spacing of the open mill is set to be 3mm, the rotating speed of the open mill is set to be 30r/min, the glue discharging temperature is set to be 95 ℃, and the mixing time of the open mill is set to be 700 seconds, so that the environment-friendly all-steel transition layer glue is obtained.
Comparative example 1
The environment-friendly all-steel transition layer adhesive comprises the following components in parts by weight: 100 parts of natural rubber, 53 parts of carbon black N326, 7 parts of zinc oxide, 2 parts of 204 tackifying resin, 1.5 parts of modified methyl methacrylate resin 396, 2 parts of anti-aging agent 4020, 1 part of anti-aging agent RD, 0.4 part of cobalt boroacylate, 5 parts of adhesive RA65, 1.3 parts of accelerator DZ, 4.2 parts of insoluble sulfur powder OT-20 and 0.2 part of scorch retarder CTP.
The preparation method of the environment-friendly all-steel transition layer rubber adopts a one-step continuous low-temperature mixing (OMS low-temperature mixing) process, and comprises the following steps:
mixing master batch by an internal mixer: putting natural rubber, carbon black N326, zinc oxide, 204 tackifying resin, modified methyl resin 396, an anti-aging agent 4020, an anti-aging agent RD and cobalt boroacylate into an internal mixer for mixing, wherein the top plug pressure is 18MPa, the rotor speed is 45r/min, the rubber discharge temperature is 150 ℃, and the time is 140s, so as to obtain a master batch;
mixing the final rubber mixing with an open mill: and (2) directly conveying the master batch obtained in the step (1) to an open mill for supplementary mixing and cooling, when the temperature of the glue is less than or equal to 75 ℃, putting an adhesive RA65, an accelerant DZ, insoluble sulfur powder OT-20 and an anti-scorching agent CTP into the open mill for mixing, wherein the roll spacing of the open mill is set to be 3mm, the rotating speed of the open mill is set to be 30r/min, the glue discharging temperature is set to be 95 ℃, and the mixing time of the open mill is set to be 700 seconds, so that the environment-friendly all-steel transition layer glue is obtained.
Comparative example 2
The environment-friendly all-steel transition layer adhesive comprises the following components in parts by weight: 100 parts of natural rubber, 53 parts of carbon black N326, 7 parts of zinc oxide, 2 parts of 204 tackifying resin, 1.5 parts of resorcinol, 2 parts of anti-aging agent 4020, 1 part of anti-aging agent RD, 0.4 part of cobalt boracylate, 5 parts of adhesive RA65, 1.3 parts of accelerator DZ, 4.2 parts of insoluble sulfur powder OT-20 and 0.2 part of scorch retarder CTP.
A preparation method of an environment-friendly all-steel transition layer adhesive comprises the following steps:
first-stage mixing: putting natural rubber, carbon black N326, zinc oxide, 204 tackifying resin and an anti-aging agent 4020 into an internal mixer for mixing, wherein the upper top plug pressure is 18MPa, the rotor rotation speed is 45r/min, the rubber discharge temperature is 155 ℃, and the time is 155s, so as to obtain a section of rubber compound;
and (3) second-stage mixing: putting the first-stage rubber compound obtained in the step (1), carbon black RD, resorcinol and cobalt boroacylate into an internal mixer for mixing, wherein the top plug pressure is 18MPa, the rotor rotation speed is 40r/min, the rubber discharge temperature is 145 ℃, and the time is 110s, so as to obtain a second-stage rubber compound;
three-stage mixing: and (3) putting the two-stage rubber compound obtained in the step (2), the adhesive RA65, the accelerant DZ, the insoluble sulfur powder OT-20 and the scorch retarder CTP into an internal mixer for mixing, wherein the rotating speed of a rotor is 25r/min, the top plug pressure is 16MPa, the rubber discharging temperature is 100 ℃, and the time is 120s, so that the environment-friendly all-steel transition layer rubber is obtained.
The environment-friendly all-steel transition layer rubber obtained in the embodiments 1-3 and the comparative example 1 is vulcanized, wherein the vulcanization conditions are as follows: the physical property test parameters of the vulcanized rubber obtained at 151 ℃ for 30 minutes are shown in Table 1.
TABLE 1 physical properties of environmental-friendly all-steel transition layer rubber after vulcanization
From the physical property test results shown in table 1, it can be seen that: in the environment-friendly all-steel transition layer rubber, the tear strength, the steel wire drawing force and the stress at definite elongation of the rubber material in the embodiment 1-2 are all improved compared with those in the comparative example 1-2, the heat generation of the rubber material is reduced, and the transition layer rubber in the embodiment 1-2 has better steel wire adhesive force after being aged. The performances can effectively improve the performances of the transition layer rubber material, and further prolong the service life of the tire.
Through the comparison of the performances of the rubber materials in the example 1 and the comparative example 1, the application of the carbon nano tube can improve the tear resistance and reduce the heat generation of the transition layer rubber; the performance comparison of the rubber materials of example 2 and comparative example 2 shows that the carbon nano tube and the modified meta-methyl resin have synergistic effect to improve the adhesive force of the transition layer rubber after aging.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. The environment-friendly all-steel transition layer adhesive is characterized by comprising the following components in parts by weight: 100 parts of natural rubber, 50-60 parts of carbon black, 0.1-3 parts of carbon nano tubes, 3-8 parts of zinc oxide, 1-4 parts of tackifying resin, 0.5-2 parts of modified methyl methacrylate resin, 1-3 parts of anti-aging agent, 0.2-1 part of cobalt salt, 652-6 parts of adhesive, 0.5-2 parts of accelerator DZ, 3-7 parts of insoluble sulfur powder and 0.1-0.5 part of anti-scorching agent CTP.
2. The environment-friendly all-steel transition layer adhesive according to claim 1, wherein the carbon black is one or both of N330 and N326.
3. The environment-friendly all-steel transition layer adhesive according to claim 1, wherein the carbon nanotubes are vapor-phase-precipitation multi-wall-agglomerated carbon nanotubes with a tube diameter of 12-15 nm, a length of 3-10 μm, and a specific surface area of 250-290 m2/g。
4. The environment-friendly all-steel transition layer adhesive as claimed in claim 1, wherein the modified meta-methyl resin is prepared by polymerization reaction of resorcinol, dicyclopentadiene and formaldehyde, and specifically comprises at least one compound represented by formula (I), formula (II) and formula (III), and has the following chemical formula:
in the formulae (I), (II) and (III), n is a natural number other than 0, and R is-CH (CH)3)C5H5Or H.
5. The environment-friendly all-steel transition layer adhesive according to claim 1, wherein the cobalt salt is cobalt boroacylate or cobalt neodecanoate.
6. The environment-friendly all-steel transition layer adhesive according to claim 1, wherein the tackifying resin is one or two of C5 tackifying resin, 203 tackifying resin and 204 tackifying resin.
7. The environment-friendly all-steel transition layer adhesive as claimed in claim 1, wherein the anti-aging agent is two or three of an anti-aging agent 4020, an anti-aging agent RD and an anti-aging agent 3100.
8. The environment-friendly all-steel transition layer adhesive according to claim 1, wherein the insoluble sulfur IS insoluble sulfur OT-20 or insoluble sulfur IS 6033.
9. The preparation method of the environment-friendly all-steel transition layer adhesive as claimed in claim 1 is characterized in that a one-step continuous low-temperature mixing process is adopted, and the preparation method comprises the following steps:
(1) mixing master batch by an internal mixer: putting 100 parts of natural rubber, 50-60 parts of carbon black, 0.1-3 parts of carbon nano tubes, 3-8 parts of zinc oxide, 1-4 parts of tackifying resin, 0.5-2 parts of modified methyl resin, 1-3 parts of anti-aging agent and 0.2-1 part of cobalt salt into an internal mixer for mixing, wherein the upper top plug pressure is 6-18 MPa, the rotor speed is 40-50 r/min, the rubber discharge temperature is 140-155 ℃, and the time is 135-160 s, so as to obtain masterbatch;
(2) mixing the final rubber mixing with an open mill: directly conveying the masterbatch obtained in the step (1) to an open mill for supplementary mixing and cooling, when the temperature of the masterbatch is less than or equal to 75 ℃, putting 2-6 parts of an adhesive RA65, 0.5-2 parts of an accelerant DZ, 3-7 parts of insoluble sulfur powder and 0.1-0.5 part of an anti-coking agent CTP into the open mill for mixing, controlling the roll spacing of the open mill to be 2.5-4 mm, controlling the rotating speed of the open mill to be 20-40 r/min, controlling the rubber discharge temperature to be 85-100 ℃, controlling the mixing time of the open mill to be 600-800 seconds, and obtaining the environment-friendly all-steel transition layer rubber after mixing.
10. The method for preparing environment-friendly all-steel transition layer rubber according to claim 9, wherein a GK320E internal mixer is adopted in the internal mixer in the step (1), and a phi 660X 2130mm open mill is adopted in the open mill in the step (2).
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