CN114347528A - Finished tire and preparation method thereof - Google Patents
Finished tire and preparation method thereof Download PDFInfo
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- CN114347528A CN114347528A CN202111417597.6A CN202111417597A CN114347528A CN 114347528 A CN114347528 A CN 114347528A CN 202111417597 A CN202111417597 A CN 202111417597A CN 114347528 A CN114347528 A CN 114347528A
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Abstract
The invention provides a finished tire and a preparation method thereof. The preparation method comprises the following steps: carrying out first vulcanization treatment on the mixed rubber material to obtain a tread half part; performing second vulcanization treatment and first molding treatment on the mixed rubber material to obtain a molded tire body; carrying out third vulcanization treatment and second molding treatment on the tread semi-part and the molded tire body to obtain a finished tire; the temperature of the first vulcanization treatment is lower than that of the second vulcanization treatment, and the weight ratio of the tread half part to the molded tire body is (20-40): 100. The tread half part is thin, the first vulcanization treatment temperature is low, and the mixed rubber material has enough time to flow in the mold, so that the tread half part can be tightly combined with a formed tire body in the third vulcanization process, and the problems of cracking of a formed joint and rubber shortage of a finished tire are avoided. The process of forming the tread half components does not involve a molding process, which can reduce instances of stiffening of the tread half components and also avoid difficulties in conforming the tread half components to the molded carcass.
Description
Technical Field
The invention relates to the technical field of finished tire preparation, in particular to a finished tire and a preparation method thereof.
Background
The wear resistance of finished all-steel truck radial tires is an important factor in the service life of the tires, and has become one of the most concerned issues in the tire technology field. In the field of all-steel wear resistance, a large amount of Natural Rubber (NR) is used, and has good elasticity and good bending and flexing resistance, but has poor heat resistance and fatigue resistance. In summer with higher temperature, the wear resistance of the tread made of all natural rubber is obviously reduced. To solve the above problems, researchers have increasingly focused their eyes on synthetic rubber, one of which is trans-isoprene rubber (TPI), an isomer of natural rubber.
Trans-isoprene rubber (often referred to as gutta percha) is a synthetic rubber material having low dynamic heat generation, low rolling resistance, and excellent wear resistance and dynamic fatigue resistance. However, due to the structural particularity, trans-isoprene rubber contains regular trans-1, 4 structure, which makes trans-isoprene rubber easy to crystallize at normal temperature, and is a crystalline thermoplastic elastomer. When the temperature exceeds 60 ℃, the trans-isoprene rubber exhibits high elasticity of the rubber.
Researchers have attempted to blend natural rubber with trans-isoprene rubber to improve the high temperature and wear resistance of the finished tire. The trans-isoprene rubber and the natural rubber are blended under the conventional conditions, the micro-uniform dispersion is difficult to achieve, the viscosity of the rubber material is poor after the trans-isoprene rubber is used, the rubber material becomes hard when the blended rubber material is stored at normal temperature, the adhesion of a subsequent forming joint is not facilitated, the problem of rubber shortage of a finished tire due to poor rubber material fluidity is solved, and the abrasion performance of the finished tire is finally influenced.
The prior patent (No. CN101550245B) provides an all-steel radial truck tire and a mixing and gelling step thereof. The preparation method of the pre-blended raw rubber in the steps comprises the following steps: when the temperature of the internal mixer reaches the initial temperature of more than 100 ℃, adding 100kg of TPI rubber, when the temperature of the mixing chamber of the internal mixer reaches more than 115 ℃, lifting the upper bolt, adding 100kg of NR rubber, pressing the upper bolt, and continuously mixing to prepare the pre-blended raw rubber with the ratio of TPI/NR being 1:1. It is thus understood that the trans-isoprene rubber and the natural rubber are blended in a weight ratio of 1:1, and TPI is charged when the internal mixer starting temperature is 100 ℃ or higher at the start of the premixing, in order to preplasticize the TPI. Although the method can realize blending and dispersing of the eucommia rubber and the natural rubber, the method has high requirements on equipment, long standby time and large energy consumption.
The prior document (publication number CN107216499A) provides a formula sizing material of an all-steel ultra-wear-resistant tread rubber and a preparation method thereof. The preparation method comprises the steps of adopting a three-section primary smelting process and a one-section final smelting process to finally obtain the all-steel ultra-wear-resistant tread rubber material, wherein the tread forming process adopts a hot fitting process, namely, the tread of the existing forming machine is supplied with rubber and is extruded by a cold feeding extruder, the extruded tread passes through a roller cooling line, the temperature of a tread part is controlled to be 40-50 ℃, and the tread is fitted to a belt ply of an auxiliary drum. Although the method solves the problem that half parts are hardened in the forming process, the control process is relatively complex, the production efficiency is low, and the method is not beneficial to energy conservation, consumption reduction and large-scale popularization.
On the basis, a method for preventing the rubber material from hardening easily, improving the flowability and improving the viscosity of the rubber material in the process of banburying and manufacturing the tire is researched and developed, and the method has important significance for solving the problem of rubber shortage of the finished tire and improving the comprehensive mechanical properties such as the wear resistance of the finished tire.
Disclosure of Invention
The invention mainly aims to provide a finished tire and a preparation method thereof, and aims to solve the problem that the conventional finished tire is easy to harden and has insufficient viscosity and poor flowability to cause the rubber shortage of the finished tire in the processes of banburying of rubber, vulcanization and forming of the finished tire.
In order to achieve the above object, an aspect of the present invention provides a method of manufacturing a finished tire, the method comprising: carrying out first vulcanization treatment on the mixed rubber material to obtain a tread half part; performing second vulcanization treatment and first molding treatment on the mixed rubber material to obtain a molded tire body; carrying out third vulcanization treatment and second molding treatment on the tread semi-part and the molded tire body to obtain a finished tire; the temperature of the first vulcanization treatment is lower than that of the second vulcanization treatment, and the weight ratio of the tread half part to the molded tire body is (20-40): 100.
Further, the first vulcanization treatment process further includes: adding a first vulcanizing agent in the first vulcanizing treatment process, and carrying out first vulcanizing treatment on the mixed rubber material and the first vulcanizing agent in a first mold to obtain a tread half part; preferably, the temperature of the first vulcanization treatment is 130-155 ℃, the pressure is 13-20 MPa, and the time is 0.5-1.2 h.
Further, the second sulfurizing treatment further comprises: adding a second vulcanizing agent in the second vulcanizing treatment process, and performing second vulcanizing treatment and first molding treatment on the mixed rubber material and the second vulcanizing agent in a second mold to obtain a molded tire body; preferably, the temperature of the second sulfurization treatment is 130-180 ℃, the pressure is 2-4 MPa, and the time is 0.5-1.0 h.
Further, the third sulfidation treatment also includes: adding a third vulcanizing agent in the third vulcanizing treatment process, and carrying out third vulcanizing treatment and third molding treatment on the tread half part, the molded tire body and the third vulcanizing agent in a third mold to obtain a finished tire; preferably, the temperature of the third sulfurization treatment is 100-130 ℃, the pressure is 400-800 kPa, and the time is 2.0-4.0 h.
Further, the preparation method of the mixed rubber compound comprises the following steps: preheating trans-isoprene rubber; in a first mixing device, performing primary mixing treatment on natural rubber, the preheated trans-isoprene rubber, a vulcanization activator and a first filler to obtain primary mixed rubber; in a second mixing device, performing two-stage mixing treatment on the first-stage mixing rubber and a second filler to obtain a second-stage mixing rubber; and finally, in a third mixing device, performing final mixing treatment on the two-stage mixed rubber, the third vulcanizing agent and the accelerator to obtain mixed rubber.
Further, the temperature of the preheating treatment is 60-110 ℃, and the time is 1-4 h; preferably, the temperature of the first mixing treatment is the same as the temperature of the preheating treatment.
Further, in the first mixing treatment process, the weight ratio of the natural rubber, the preheated trans-isoprene rubber, the vulcanization activator and the first filler is (75-80): 20-25): 6-6.5): 33-37.5); preferably, the number average molecular weight of the natural rubber is 20-30W, and the molecular weight distribution index is 4-5; the trans-isoprene rubber has a number average molecular weight of 7-30W and a molecular weight distribution index of 4-7.
Further, the preparation method of the mixed rubber material also comprises the following steps: in the process of one-stage mixing treatment, tackifying resin, anti-aging agent and plasticizer are added; preferably, the weight ratio of the natural rubber, the tackifying resin, the anti-aging agent and the plasticizer is (75-80): 1-2): 2.5-3.0): 1.0-2.0.
Further, the first filler and the second filler are each independently selected from carbon black and/or white carbon; preferably, the weight ratio of the first filler to the second filler is (33-37.5): 12.5-21.
Further, the preparation method of the mixed rubber material also comprises the following steps: adding an anti-coking agent in the process of final refining treatment; preferably, the weight ratio of the second-stage rubber compound, the third vulcanizing agent, the accelerator and the scorch retarder is 100 (0.7-0.9): (0.6-0.7): 0.06-0.09).
Further, when the first filler and/or the second filler is/are carbon black and white carbon black, the preparation method of the mixed rubber material further comprises the following steps: adding a coupling agent in the process of two-stage mixing treatment; preferably, the weight ratio of the first-stage rubber compound to the coupling agent is 100 (1.0-1.8).
In another aspect, the present invention provides a finished tire obtained by the method for preparing the finished tire.
According to the technical scheme, the mixed rubber is vulcanized to form a tread half part through first vulcanization treatment, meanwhile, the mixed rubber is sequentially subjected to second vulcanization treatment and first molding treatment to form a molded tire body, and then third vulcanization treatment and second molding treatment are carried out on the tread half part with specific weight and the molded tire body with specific weight, so that a finished tire with a thin tread is obtained. Because the tread half part is thin and the temperature of the first vulcanization treatment is low, the mixed rubber material has enough time to flow in the mold, so that the mixed rubber material can be tightly combined with a formed tire body in the third vulcanization process, and the problems of cracking of a formed joint and rubber shortage of a finished tire are further avoided. In the preparation process of the finished tire, the process of forming the tread half part only involves vulcanization crosslinking reaction and does not involve a forming process, so that the condition that the tread half part is hardened can be greatly reduced, and meanwhile, the quality problems that the forming joint is cracked and the like caused by difficult fitting between the tread half part and a formed tire body and insufficient viscosity of the tread half part in the subsequent second forming treatment are also avoided. In addition, the preparation method can realize continuous production, and has simple control process and low production cost.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a photograph of a finished tire made in example 1 of the present invention; and
fig. 2 shows a photograph of a finished tire according to comparative example 1 of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background of the invention, the prior finished tire has the problems of easy hardening of the rubber material, insufficient viscosity and poor flowability during the banburying of the rubber material, the vulcanization of the finished tire and the molding process, which results in the rubber shortage of the finished tire. In order to solve the technical problem, the application provides a preparation method of a finished tire. The preparation method of the finished tire comprises the following steps: carrying out first vulcanization treatment on the mixed rubber material to obtain a tread half part; performing second vulcanization treatment and first molding treatment on the mixed rubber material to obtain a molded tire body; carrying out third vulcanization treatment and second molding treatment on the tread semi-part and the molded tire body to obtain a finished tire; the temperature of the first vulcanization treatment is lower than that of the second vulcanization treatment, and the weight ratio of the tread half part to the molded tire body is (20-40): 100.
And vulcanizing the mixed rubber material to form a tread half part by adopting the first vulcanization treatment, simultaneously forming a molded tire body by sequentially carrying out second vulcanization treatment and first molding treatment on the mixed rubber material, and carrying out the third vulcanization treatment and the second molding treatment on the tread half part with specific weight and the molded tire body with specific weight to obtain a finished tire with a thinner tread. Because the tread half part is thin and the temperature of the first vulcanization treatment is low, the mixed rubber material can flow in the mold for enough time, so that the mixed rubber material can be tightly combined with a formed tire body in the third vulcanization process, and the problems of cracking of a formed joint and rubber shortage of a finished tire are further avoided. In the preparation process of the finished tire, the process of forming the tread half part only involves vulcanization crosslinking reaction and does not involve a forming process, so that the condition that the tread half part is hardened can be greatly reduced, and meanwhile, the quality problems that the forming joint is cracked and the like caused by difficult fitting between the tread half part and a formed tire body and insufficient viscosity of the tread half part in the subsequent second forming treatment are also avoided. In addition, the preparation method can realize continuous production, and has simple control process and low production cost.
In a preferred embodiment, the first vulcanization process further comprises: and adding a first vulcanizing agent in the first vulcanizing treatment process, and carrying out first vulcanizing treatment on the mixed rubber compound and the first vulcanizing agent in a first mold to obtain the tread half part. The first vulcanization treatment can enable the mixed rubber to be crosslinked, and the tread semi-part formed after crosslinking can avoid the problem that the finished tire joint is cracked due to insufficient viscosity of the tread joint.
In order to accurately control the degree of crosslinking of the mixed rubber material and enable the mixed rubber material to flow in the first mold for a sufficient time to improve the fluidity and viscosity of the mixed rubber material, thereby being beneficial to inhibiting the occurrence of the poor condition of rubber shortage of the tire tread, the temperature of the first vulcanization treatment is preferably 130-155 ℃, the pressure is preferably 13-20 MPa, and the time is preferably 0.5-1.2 h.
In a preferred embodiment, the second sulfurizing process further comprises: and adding a second vulcanizing agent in the second vulcanizing treatment process, and performing second vulcanizing treatment and first molding treatment on the mixed rubber material and the second vulcanizing agent in a second mold to obtain a molded tire body. The molded tire body is obtained after the second vulcanization treatment and the first molding treatment, and the molded tire body obtained after the vulcanization crosslinking reaction and the molding treatment has a three-dimensional crosslinking network structure inside, so that the strength is better, the molded tire body and the half part of the tire tread are tightly combined in the preparation process of a subsequent finished tire, and the problems of cracking of a molded joint and rubber shortage of the finished tire are further avoided.
In order to obtain a molded tire body with a specific three-dimensional cross-linked network structure, the second vulcanization treatment temperature is preferably 130-180 ℃, the pressure is preferably 2-4 MPa, and the time is preferably 0.5-1 h.
In a preferred embodiment, the third sulfidation treatment further comprises: and adding a third vulcanizing agent in the third vulcanizing process, and carrying out third vulcanizing treatment on the tread half part, the molded tire body and the third vulcanizing agent in a third mold to obtain a finished tire. Adopt above-mentioned third vulcanization to handle and can make half parts of tread and moulded carcass take place the crosslinking, be favorable to making half parts of tread and moulded carcass combine inseparabler, simultaneously, half parts of tread do not relate to the shaping process, avoided because half parts of tread turn hard, avoided laminating difficulty and half parts of tread viscidity not enough to lead to the quality problems such as shaping joint fracture when the shaping.
In order to enable the tread half part and the formed tire body to have a crosslinking reaction more thoroughly and greatly reduce the occurrence of the phenomenon of rubber shortage on the surface of the finished tire, the temperature of the third vulcanization treatment is preferably 100-130 ℃, the pressure is preferably 400-800 kPa, and the time is 2.0-4.0 h.
In a preferred embodiment, the process for preparing the compounded composition comprises: preheating trans-isoprene rubber; in a first mixing device, performing primary mixing treatment on natural rubber, the preheated trans-isoprene rubber, a vulcanization activator and a first filler to obtain primary mixed rubber; in a second mixing device, performing two-stage mixing treatment on the first-stage mixing rubber and a second filler to obtain a second-stage mixing rubber; and finally, in a third mixing device, performing final mixing treatment on the two-stage mixed rubber, the third vulcanizing agent and the accelerator to obtain mixed rubber.
Through carrying out the preheating treatment on the trans-isoprene rubber, the mobility of the preheated trans-isoprene rubber is higher than that of the trans-isoprene rubber, so that on one hand, the compatibility and the dispersion uniformity of the natural rubber and the trans-isoprene rubber are greatly improved, and the synergistic effect of the natural rubber and the trans-isoprene rubber is improved, on the other hand, the processability of a mixed rubber material is improved, the subsequent addition of a first filler and a second filler is facilitated, and further, the improvement of the comprehensive mechanical properties such as the wear resistance, the fatigue resistance and the like of a subsequently prepared finished tire is facilitated. Compared with single batch addition, the first filler and the second filler are added in the first-stage mixing treatment and the second-stage mixing treatment respectively, so that the dispersibility of the first filler and the second filler in a mixing system is improved, the addition amount of the first filler and the second filler is further improved, and the comprehensive mechanical properties such as the wear resistance and the like of a finished tire prepared subsequently are improved.
The trans-isoprene rubber contains a regular trans-1, 4 structure, so that the trans-isoprene rubber is easy to crystallize at normal temperature and is a crystalline thermoplastic elastomer. When the temperature exceeds 60 ℃, the trans-isoprene rubber exhibits high elasticity of the rubber. In a preferred embodiment, the temperature of the preheating treatment is 60-110 ℃ and the time is 1-4 h. The temperature and time of the pre-heat treatment include, but are not limited to, the above ranges, and the limitation of the temperature and time within the above ranges is beneficial to improve the fluidity of the trans-isoprene rubber and the compatibility with the natural rubber, thereby being beneficial to further improve the processability of the mixed rubber compound.
In a preferred embodiment, the temperature of the first mixing step is the same as the temperature of the preheating step. Limiting the temperature of the first-stage mixing treatment and the temperature of the preheating treatment to be the same temperature is beneficial to further improving the compatibility and the dispersion uniformity of the natural rubber and the trans-isoprene rubber, and simultaneously, inhibiting additional heat conduction caused by different temperatures and keeping the constant temperature of the first-stage mixing system.
Specifically, the first-stage mixing treatment comprises: adding the preheated trans-isoprene rubber into a first mixing device, setting the rotating speed of the first mixing device to be 40-50 r/min, setting the temperature of the first mixing device to be the same as the temperature of the preheating treatment, pressing a top bolt for 10-20 s, and lifting the top bolt to be in place; adding a vulcanization activator and a first filler into a first mixing device, and starting a first mixing treatment; pressing the top bolt for 25-35 s, lifting the top bolt for cleaning, pressing the top bolt for 20-30 s, lifting the top bolt to the proper position, and pressing the top bolt for 15-25 s; performing first rubber discharge treatment on the material in the first mixing device to obtain a section of mixed rubber; the temperature of the first glue discharging treatment is 160-170 ℃. Preferably, the one-stage mixing process further comprises: adding tackifying resin, an anti-aging agent and a plasticizer into a first mixing device, and starting a first mixing treatment.
In a preferred embodiment, the weight ratio of the natural rubber, the preheated trans-isoprene rubber, the vulcanization activator and the first filler in the first mixing step is (75-80): (20-25): (6-6.5): (33-37.5). The weight ratio of the natural rubber, the preheated trans-isoprene rubber, the vulcanization activator and the first filler includes but is not limited to the above range, and the restriction of the weight ratio to the weight ratio is favorable for reducing the rolling resistance of a subsequently prepared finished tire, so that the wear resistance of the finished tire is improved; meanwhile, the dynamic heat generation of the steel is reduced, and the fatigue resistance of the steel is improved.
The addition of the vulcanization activator can improve the activity of the accelerator and shorten the vulcanization time. The vulcanization activator employed herein includes, but is not limited to, stearic acid and/or zinc oxide.
In order to further reduce the rolling resistance of the finished tire and improve the wear resistance of the finished tire; meanwhile, in order to further reduce the dynamic heat generation of the finished tire and improve the fatigue resistance of the finished tire, the number average molecular weight of the natural rubber is preferably 20-30W, and the molecular weight distribution index is preferably 4-5; the trans-isoprene rubber has a number average molecular weight of 7-30W and a molecular weight distribution index of 4-7.
In order to improve the processability of the mixed rubber compound and the aging resistance of the finished tire obtained subsequently, in a preferred embodiment, the preparation method of the mixed rubber compound further comprises the following steps: in the process of one-stage mixing treatment, tackifying resin, anti-aging agent and plasticizer are added.
In order to further improve the processing performance of the mixed rubber material and the comprehensive performance such as aging resistance of a finished tire prepared subsequently, the weight ratio of the natural rubber, the tackifying resin, the anti-aging agent and the plasticizer is preferably (75-80): 1-2): 2.5-3.0 ]: 1.0-2.0.
The tackifying resins employed herein include, but are not limited to, one or more of the group consisting of acetylenic tertiary butyl phenol formaldehyde super tackifying resin KORESIN, tertiary butyl phenol formaldehyde tackifying resin, and octylphenol formaldehyde tackifying resin; the anti-aging agent adopted by the application comprises one or more of the group consisting of but not limited to anti-aging agent 4020, anti-aging agent RD and anti-aging agent 3100; plasticizers useful herein include, but are not limited to, plasticizer a and/or zinc soap salts.
Specifically, the two-stage kneading treatment includes: setting the rotating speed of a second mixing device to be 35-45 r/min, adding a section of mixing rubber and a second filler into the first mixing device, pressing a top bolt for 25-35 s, lifting the top bolt for cleaning, pressing the top bolt for 15-25 s, lifting the top bolt to be in place, and pressing the top bolt for 15-25 s; performing second rubber discharge treatment on the material in the first mixing device to obtain a second-stage mixed rubber; the temperature of the second glue discharging treatment is 150-170 ℃. Preferably, the two-stage mixing process further comprises: the coupling agent is added to the first mixing device and the two-stage mixing process is started.
In a preferred embodiment, the first filler and the second filler each independently include, but are not limited to, carbon black and/or white carbon. The use of the above preferred types of first and second fillers is advantageous in improving the wear resistance of the finished tire compared to other types.
In order to further improve the dispersion uniformity of the first filler and the second filler in the kneading system, the weight ratio of the first filler to the second filler is preferably (33-37.5): (12.5-21).
Specifically, the final processing comprises: setting the rotating speed of a third mixing device to be 20-30 r/min, adding the two-stage rubber compound, a third vulcanizing agent and an accelerator into a second mixing device, pressing a top bolt for 25-35 s, lifting the top bolt for cleaning, pressing the top bolt for 20-30 s, lifting the top bolt in place, and pressing the top bolt for 15-25 s; performing third glue discharging treatment to obtain a glue material; preferably, the temperature of the third glue discharging treatment is 95-105 ℃; preferably, the finishing process further comprises: and adding the second-stage rubber compound, the third vulcanizing agent, the accelerator and the anti-coking agent into a second mixing device, and starting final mixing treatment.
In a preferred embodiment, the first mixing apparatus, the second mixing apparatus and the third mixing apparatus each independently include, but are not limited to, different types of internal mixers. For example, an F305 internal mixer, an F270 internal mixer, an F370 internal mixer, and a GK255 internal mixer can be used.
The addition of the scorch retarder can reduce the possibility of scorching of the vulcanization system during the final refining treatment. In a preferred embodiment, the method for preparing the mixed rubber compound further comprises the following steps: during the final refining process, an anti-scorching agent is added. In order to further control the degree of the final refining process and reduce the possibility of scorching, the weight ratio of the second-stage rubber compound, the third vulcanizing agent, the accelerating agent and the scorch retarder is preferably 100 (0.7-0.9): (0.6-0.7): 0.06-0.09).
The addition of the coupling agent can improve the degree of coupling reaction between the rubber compound and the second filler, which is beneficial to improving the crosslinking density and further improving the wear resistance of the finished rubber. In a preferred embodiment, when the first filler and/or the second filler is carbon black and white carbon, the method for preparing the mixed rubber compound further comprises: in the process of two-stage mixing treatment, a coupling agent is added. In order to further improve the crosslinking density and further improve the wear resistance of the finished rubber, the weight ratio of the first-stage rubber compound to the coupling agent is preferably 100 (1.0-1.8).
The scorch retarder employed herein includes, but is not limited to, one or more of the group consisting of the scorch retarder CTP and the scorch retarder CTP-80; the promoters employed herein include, but are not limited to, one or more of the group consisting of promoter NS, promoter CZ, and promoter DZ; the first, second and third vulcanizing agents employed herein each independently include, but are not limited to, one or more of the group consisting of sulfur, insoluble sulfur OT 20, insoluble sulfur 6033 and insoluble sulfur OT 10.
The second aspect of the present application further provides a finished tire, which is prepared by the preparation method of the finished tire provided by the present application. The application provides a finished product child does not have the problem of starving for glue, and the wastrel of finished product child is few.
It should be noted that, in all the examples and comparative examples of the present application, the following methods are used for each test, specifically:
carrying out processability test on the mixed rubber material, wherein the Mooney viscosity is tested according to GB/T1232.1-2016 under the test condition of 125 ℃; the initial vulcanization characteristic of the unvulcanized rubber is tested according to GB/T1233-2008;
and (3) performing mechanical test on the mixed rubber material after vulcanization at 150 ℃ for 30min, and testing the tensile stress strain performance at room temperature according to GB/T528-2009.
The filler dispersity of the mixed rubber is tested according to GB/T6030-2006, and the test condition is 150 ℃ multiplied by 30 min.
The DMA test (dynamic thermomechanical analysis test) was carried out on the compounded rubber compound by using a GABO dynamic thermomechanical analyzer under the conditions of a tensile mode, a static strain of 7%, a dynamic strain of 0.25%, and a frequency of 10Hz, and the test result was represented by tan. delta. @60 ℃.
The wear resistance is tested according to GB/T1689-.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
The natural rubber used in example 1 had a number average molecular weight of 23W and a molecular weight distribution index of 4.7; the trans-isoprene rubber has a number average molecular weight of 7-30W and a molecular weight distribution index of 5.0.
A preparation method of mixed rubber comprises the following steps:
preheating treatment: the trans-isoprene rubber was subjected to a preheating treatment at 80 ℃ for 2 hours.
First-stage mixing treatment: setting the rotation speed of an F305 internal mixer to be 45r/min, adding natural rubber into the F305 internal mixer, mixing to 80 ℃, adding preheated trans-isoprene rubber, pressing a top bolt for 15s, lifting the top bolt to a proper position, adding a first filler of carbon black N134, a vulcanization activator zinc oxide, stearic acid, acetylene type tert-butyl phenolic super tackifying resin KORESIN, an anti-aging agent 4020 and an anti-aging agent RD into the F305 internal mixer, pressing the top bolt for 30s, lifting the top bolt for cleaning, pressing the top bolt for 25s, lifting the top bolt to a proper position, pressing the top bolt for 20s, opening a discharge gate to discharge rubber, and controlling the temperature of first rubber discharge treatment to be 165 ℃; and (4) discharging the rubber pieces by using an open mill, and cooling to obtain a first-stage rubber compound. In the first mixing treatment process, the weight ratio of the natural rubber, the preheated trans-isoprene rubber, the zinc oxide, the stearic acid and the carbon black N134 is 80:20:4:2: 37.5; the weight portion ratio of the natural rubber, the tackifying resin KORESIN, the anti-aging agent 4020 and the anti-aging agent RD is 80:1:1.5: 1.
And (3) secondary mixing treatment: setting the rotating speed of an F305 internal mixer to be 40r/min, simultaneously adding the prepared rubber compound and a second filler of carbon black N134 into the F305 internal mixer, pressing a top bolt for 30s, lifting the top bolt to clean, pressing the top bolt for 20s, lifting the top bolt to be in place, pressing the top bolt for 20s, opening a discharging door to discharge rubber, and controlling the temperature of rubber discharge treatment to be 165 ℃; and (4) discharging the rubber pieces by using an open mill, and cooling to obtain a two-stage rubber compound. The weight ratio of the first-stage rubber compound to the second filler of carbon black N134 is 100:8.5, and the weight ratio of the second filler of carbon black N134 to the first filler of carbon black N134 is 1: 3.
Final refining treatment: setting the rotating speed of an F270 internal mixer to be 25r/min, adding the prepared two-stage rubber compound, a third vulcanizing agent sulfur, an accelerator NS and an anti-scorching agent CTP into the F270 internal mixer, pressing a top bolt for 30s, lifting the top bolt for cleaning, pressing the top bolt for 25s, lifting the top bolt to be in place, pressing the top bolt for 20s, discharging rubber from a discharge door, controlling the temperature of rubber discharging treatment to be 100 ℃, discharging the rubber from a mixer, and cooling to obtain the mixed rubber material. The weight ratio of the second-stage rubber compound to the third vulcanizing agent to the accelerator to the scorch retarder is 100:0.9:0.6: 0.09.
The above prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 1.
A method of making a finished tire, comprising:
and carrying out first vulcanization treatment on the mixed rubber material, wherein the temperature of the first vulcanization treatment is 135 ℃, the pressure is 18MPa, and the time is 0.7h, so as to obtain the tread half part.
And performing second vulcanization treatment and first molding treatment on the mixed rubber material, wherein the temperature of the second vulcanization treatment is 150 ℃, the pressure is 3MPa, and the time is 1h, and the molded tire body is obtained after the treatment.
And carrying out third vulcanization treatment on the obtained tread semi-part and the formed tire body, wherein the temperature of the third vulcanization treatment is 125 ℃, the pressure is 600kPa, and the time is 3h, so as to obtain a finished tire. The weight ratio of tread half to carcass in the finished tire was 30: 100.
The photo of the finished tire obtained in example 1 is shown in fig. 1, and it can be seen from fig. 1 that the surface of the finished tire is intact and no rubber starvation occurs.
Example 2
The difference from example 1 is that: a preparation method of mixed rubber comprises the following steps:
preheating treatment: the trans-isoprene rubber is subjected to preheating treatment at the temperature of 85 +/-5 ℃ for 2 hours.
First-stage mixing treatment: setting the rotation speed of an F305 internal mixer to be 45r/min, adding natural rubber into the F305 internal mixer, mixing to 80 ℃, adding preheated trans-isoprene rubber, pressing a top bolt for 15s, lifting the top bolt for cleaning, adding a first filler of carbon black N134, zinc oxide, a vulcanization activator stearic acid, a plasticizer A, an anti-aging agent 4020 and an anti-aging agent RD into the F305 internal mixer, pressing the top bolt for 30s, lifting the top bolt for cleaning, pressing the top bolt for 25s, lifting the top bolt to be in place, pressing the top bolt for 20s, opening a discharging door for discharging rubber, and controlling the temperature of first rubber discharging treatment to be 165-170 ℃; and (4) discharging the rubber pieces by using an open mill, and cooling to obtain a first-stage rubber compound. In the first mixing process, the weight ratio of the natural rubber, the preheated trans-isoprene rubber, the zinc oxide, the stearic acid and the carbon black N134 is 75:25:4.5:2:33, and the weight ratio of the natural rubber, the anti-aging agent 4020, the anti-aging agent RD and the plasticizer A is 75:2:1: 1.5.
And (3) secondary mixing treatment: setting the rotating speed of an F305 internal mixer to be 40r/min, simultaneously adding the prepared first-stage rubber compound, a second filler of carbon black N134, white carbon black and a coupling agent of bis- [ (gamma- (triethoxysilyl) propyl) ] tetrasulfide (abbreviated as TESPT, the brand of Germany Desmoset Si69) into the F305 internal mixer, pressing a top bolt for 30s, lifting the top bolt for cleaning, pressing the top bolt for 20s, lifting the top bolt to be in place, adjusting the rotating speed to be 30r/min, pressing the top bolt for 40s, and discharging rubber from a discharging gate, wherein the temperature of rubber discharging treatment is controlled to be 152 ℃; and (4) discharging the rubber pieces by using an open mill, and cooling to obtain a two-stage rubber compound. The weight portion ratio of the first-stage rubber compound to the second filler of carbon black N134 to the white carbon black to the coupling agent Si69 is 100:7.6:6.9:1.4, and the weight portion ratio of the second filler of carbon black N134 to the first filler of carbon black N134 is 1: 3.
Final refining treatment: setting the rotating speed of an F270 internal mixer to be 25r/min, adding the prepared two-stage rubber compound, a third vulcanizing agent sulfur, an accelerator NS and an anti-scorching agent CTP into the F270 internal mixer, pressing a top bolt for 30s, lifting the top bolt for cleaning, pressing the top bolt for 25s, lifting the top bolt to be in place, pressing the top bolt for 20s, discharging rubber from a discharge door, controlling the temperature of rubber discharging treatment to be 100 ℃, discharging the rubber from a mixer, and cooling to obtain the mixed rubber material. The weight ratio of the second-stage rubber compound to the third vulcanizing agent to the accelerator to the scorch retarder is 100:0.7:0.7: 0.06.
As shown in fig. 1, no starving of the finished tire surface occurred. The above prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 1.
Example 3
The difference from example 1 is that: the preparation method of the mixed rubber compound does not comprise preheating treatment.
The above prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 1.
Example 4
The difference from example 2 is that: the preparation method of the mixed rubber compound does not comprise preheating treatment.
The above prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 1.
TABLE 1
Example 5
The difference from example 1 is that: the temperature for carrying out the first vulcanization treatment on the mixed rubber compound and the first vulcanizing agent is 130 ℃, the pressure is 16MPa, and the time is 1.2 h.
The above prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 2.
Example 6
The difference from example 1 is that: the temperature for carrying out the first vulcanization treatment on the mixed rubber material and the first vulcanizing agent is 155 ℃, the pressure is 20MPa, and the time is 0.8 h.
The above prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 2.
Example 7
The difference from example 1 is that: the temperature for carrying out the first vulcanization treatment on the mixed rubber material and the first vulcanizing agent is 120 ℃, the pressure is 12MPa, and the time is 1.3 h.
The above prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 2.
TABLE 2
Example 8
The difference from example 1 is that: the preheating treatment temperature of the trans-isoprene rubber is 60 ℃, and the time is 4 hours.
The above-prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 3.
Example 9
The difference from example 1 is that: the preheating treatment temperature of the trans-isoprene rubber is 110 ℃, and the time is 1 h.
The above-prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 3.
Example 10
The difference from example 1 is that: the preheating treatment temperature of the trans-isoprene rubber is 120 ℃, and the time is 0.8 h.
The above-prepared compounded rubber materials were subjected to performance tests, and the test results are shown in table 3.
TABLE 3
Comparative example 1
The difference from example 1 is that: and carrying out primary vulcanization molding treatment on the mixed rubber material to obtain an unqualified finished tire. The one-step vulcanization molding process comprises the step of processing half parts such as a tire tread, a tire side, a bead filler, an air-tight layer and the like which are finished by extrusion, calendering and other post processes on a molding machine to obtain a tire blank.
As shown in fig. 2, the preparation method of comparative example 1 has difficulty in obtaining a qualified finished tire and has a significant phenomenon of surface starvation.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
comparing the embodiment 1 and the embodiment 3 respectively, and comparing the embodiment 2 and the embodiment 4, it can be seen that the mobility of the trans-isoprene rubber after the preheating treatment is higher than that of the trans-isoprene rubber by performing the preheating treatment on the trans-isoprene rubber, which is beneficial to greatly improving the compatibility and the dispersion uniformity of the natural rubber and the trans-isoprene rubber and improving the synergistic effect of the natural rubber and the trans-isoprene rubber on the one hand, and is beneficial to improving the processability of the mixed rubber material on the other hand, facilitating the addition of the subsequent first filler and the second filler, and further being beneficial to improving the comprehensive mechanical properties such as the wear resistance, the fatigue resistance and the like of the subsequently prepared finished tire. Compared with single batch addition, the first filler and the second filler are added in the first-stage mixing treatment and the second-stage mixing treatment respectively, so that the dispersibility of the first filler and the second filler in a mixing system is improved, the addition amount of the first filler and the second filler is further improved, and the comprehensive mechanical properties such as the wear resistance and the like of a finished tire prepared subsequently are improved.
Comparing examples 1, 5 to 7 with the results of the tests in Table 2, it can be seen that example 7 does not use the first vulcanization temperature, pressure and time within the preferred ranges of the present application, and that the compounded compounds obtained are inferior to examples 1, 5 and 6 in processability, filler dispersion, mechanical properties and abrasion resistance. It is understood that limiting the temperature, pressure and time of the first vulcanization process to the preferred ranges of the present application is advantageous for precisely controlling the degree of crosslinking of the kneaded compound, allowing the kneaded compound a sufficient time to flow in the first mold, improving the fluidity and viscosity thereof, and thus advantageously suppressing the occurrence of the defects of under-tread.
Comparing examples 1, 8 to 10 with the results of Table 3, it can be seen that the pre-heat treatment temperature and time used in example 10 are outside the preferred ranges of the present application and that the compounded compounds produced have inferior processability, filler dispersion, mechanical properties and abrasion resistance to examples 1, 8 and 9. It can be seen that the temperature and time of the pre-heat treatment, including but not limited to the preferred ranges, are limited to the preferred ranges, which are beneficial to improve the flowability of the trans-isoprene rubber, improve the compatibility with the natural rubber, and improve the processability of the mixed rubber compound.
Comparing example 1 with comparative example 1 and combining the object diagrams of fig. 1 and fig. 2, it can be seen that the problem of rubber shortage caused by insufficient time flowing of rubber compound can be avoided by using the above-described method for producing a finished tire provided by the present application.
It is noted that the terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those described or illustrated herein.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (12)
1. A method of manufacturing a finished tire, the method comprising:
carrying out first vulcanization treatment on the mixed rubber material to obtain a tread half part;
performing second vulcanization treatment and first molding treatment on the mixed rubber material to obtain a molded tire body;
carrying out third vulcanization treatment and second molding treatment on the tread semi-part and the molded tire body to obtain a finished tire; the temperature of the first vulcanization treatment is lower than that of the second vulcanization treatment, and the weight ratio of the tread half part to the molded tire body is (20-40): 100.
2. The method for producing a finished tire according to claim 1, wherein the first vulcanization process further includes: adding a first vulcanizing agent in the first vulcanizing treatment process, and carrying out the first vulcanizing treatment on the mixed rubber compound and the first vulcanizing agent in a first mold to obtain the tread half part;
preferably, the temperature of the first vulcanization treatment is 130-155 ℃, the pressure is 13-20 MPa, and the time is 0.5-1.2 h.
3. The method for manufacturing a finished tyre according to claim 2, wherein said second vulcanisation process further comprises: adding a second vulcanizing agent in the second vulcanizing treatment process, and performing the second vulcanizing treatment and the first molding treatment on the mixed rubber material and the second vulcanizing agent in a second mold to obtain the molded tire body;
preferably, the temperature of the second sulfurization treatment is 130-180 ℃, the pressure is 2-4 MPa, and the time is 0.5-1.0 h.
4. The method for producing a finished tyre according to any one of claims 1 to 3, wherein said third vulcanisation treatment further comprises: adding a third vulcanizing agent in the third vulcanizing process, and carrying out third vulcanizing treatment and second molding treatment on the tread half part, the molded tire body and the third vulcanizing agent in a third mold to obtain a finished tire;
preferably, the temperature of the third sulfurization treatment is 100-130 ℃, the pressure is 400-800 kPa, and the time is 2.0-4.0 h.
5. Method for producing a finished tyre according to any one of claims 1 to 4, characterized in that said mixed compound is produced by a method comprising:
preheating trans-isoprene rubber;
in a first mixing device, performing primary mixing treatment on the natural rubber, the preheated trans-isoprene rubber, the vulcanization activator and the first filler to obtain primary mixed rubber;
in the second mixing device, performing two-stage mixing treatment on the first-stage mixing rubber and a second filler to obtain a second-stage mixing rubber;
and finally mixing the two-stage rubber compound, a third vulcanizing agent and an accelerator in a third mixing device to obtain the mixed rubber material.
6. The method for preparing a finished tire according to claim 5, wherein the preheating treatment is performed at a temperature of 60-110 ℃ for 1-4 hours;
preferably, the temperature of the first mixing treatment is the same as the temperature of the preheating treatment.
7. The method for producing a finished tire according to any one of claims 5 or 6, wherein in the first-stage mixing treatment, the weight ratio of the natural rubber, the preheated trans-isoprene rubber, the vulcanization activator and the first filler is (75-80): 20-25): 6-6.5): 33-37.5;
preferably, the number average molecular weight of the natural rubber is 20-30W, and the molecular weight distribution index is 4-5; the trans-isoprene rubber has a number average molecular weight of 7-30W and a molecular weight distribution index of 4-7.
8. Method for producing a finished tyre according to any one of claims 5 to 7, characterized in that said method for producing a mixed compound further comprises: adding tackifying resin, an anti-aging agent and a plasticizer in the process of the first mixing treatment;
preferably, the weight ratio of the natural rubber, the tackifying resin, the anti-aging agent and the plasticizer is (75-80): 1-2): 2.5-3.0: 1.0-2.0.
9. The method of producing a finished tire according to claim 8, wherein the first and second fillers are each independently selected from carbon black and/or white carbon;
preferably, the weight ratio of the first filler to the second filler is (33-37.5): 12.5-21.
10. A method of producing a finished tyre according to any one of claim 9, wherein said method of producing the mixed compound further comprises: adding an anti-coking agent in the process of the final refining treatment;
preferably, the weight ratio of the second-stage rubber compound, the third vulcanizing agent, the accelerator and the scorch retarder is 100 (0.7-0.9): (0.6-0.7): 0.06-0.09).
11. The method of producing a finished tire according to claim 9 or 10, wherein when the first filler and/or the second filler is the carbon black and the white carbon, the method of producing the compounded rubber compound further comprises: adding a coupling agent in the process of the two-stage mixing treatment;
preferably, the weight ratio of the first-stage rubber compound to the coupling agent is 100 (1.0-1.8).
12. A finished tyre, characterized in that it is obtained by a method for manufacturing a finished tyre according to any one of claims 1 to 11.
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| CN102924760A (en) * | 2012-10-25 | 2013-02-13 | 北京化工大学 | High-performance tyre with ultra-wear resistant tyre surface and manufacturing method thereof |
| CN103847116A (en) * | 2012-11-30 | 2014-06-11 | 中国化工橡胶桂林有限公司 | Tire molding technology |
| CN104960388A (en) * | 2015-07-07 | 2015-10-07 | 田琬玥 | Novel tire and preparation method thereof |
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| JP2008093952A (en) * | 2006-10-11 | 2008-04-24 | Sumitomo Rubber Ind Ltd | Manufacturing method of pneumatic tire |
| CN102173067A (en) * | 2011-01-07 | 2011-09-07 | 青岛科技大学 | Novel tire molding method |
| CN102924760A (en) * | 2012-10-25 | 2013-02-13 | 北京化工大学 | High-performance tyre with ultra-wear resistant tyre surface and manufacturing method thereof |
| CN103847116A (en) * | 2012-11-30 | 2014-06-11 | 中国化工橡胶桂林有限公司 | Tire molding technology |
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