CN113172784A - Rubber final refining process for internal mixer - Google Patents

Rubber final refining process for internal mixer Download PDF

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Publication number
CN113172784A
CN113172784A CN202110498589.2A CN202110498589A CN113172784A CN 113172784 A CN113172784 A CN 113172784A CN 202110498589 A CN202110498589 A CN 202110498589A CN 113172784 A CN113172784 A CN 113172784A
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rubber
mixing
mixing chamber
internal mixer
temperature
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CN113172784B (en
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边慧光
肖鑫鑫
王禄银
许明辉
汪传生
王志飞
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Qingdao University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/002Methods
    • B29B7/005Methods for mixing in batches
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/74Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/7476Systems, i.e. flow charts or diagrams; Plants
    • B29B7/7495Systems, i.e. flow charts or diagrams; Plants for mixing rubber
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/02Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/22Component parts, details or accessories; Auxiliary operations
    • B29B7/28Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
    • B29B7/286Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control measuring properties of the mixture, e.g. temperature, density
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/80Component parts, details or accessories; Auxiliary operations
    • B29B7/82Heating or cooling
    • B29B7/823Temperature control
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/80Component parts, details or accessories; Auxiliary operations
    • B29B7/82Heating or cooling
    • B29B7/826Apparatus therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/02Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/06Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
    • B29B7/10Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
    • B29B7/18Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/183Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft having a casing closely surrounding the rotors, e.g. of Banbury type

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

The invention belongs to the technical field of rubber mixing, and relates to a rubber final mixing process for an internal mixer, which comprises the following specific steps: (1) raising the temperature of the mixing chamber to 120 ℃; (2) adding a vulcanizing agent into an internal mixing chamber, dropping a top bolt and preserving heat; (3) putting the chopped mixing rubber blocks into an internal mixing chamber; (4) after the mixing rubber block is put into the mixing chamber, the accelerator is immediately put into the mixing chamber, the ram mixing is carried out, the temperature of the mixing chamber is set to be higher, under the action of liquid sulfur, the Mooney viscosity of the rubber material is rapidly reduced, the shearing action of a rotor is reduced, meanwhile, the temperature of the whole mixing chamber can be reduced by the mixing rubber with lower temperature, the temperature is kept within a proper range, the vulcanizing agent is firstly added for melting, then the mixing rubber is put into the mixing chamber, the mixing rubber is uniformly mixed with the vulcanizing agent in the heating and plastication process, the accelerator is immediately added for mixing after the rubber feeding is finished, the vulcanizing agent and the accelerator are separately added, and the accelerator is arranged to be added at last, so that the scorching phenomenon of the rubber material can be avoided to the greatest extent.

Description

Rubber final refining process for internal mixer
The technical field is as follows:
the invention belongs to the technical field of rubber mixing, and relates to a rubber final mixing process for an internal mixer, which can improve the production efficiency.
Background art:
final mixing is an essential step in the rubber processing: adding a vulcanizing agent and an accelerant into the mixed rubber material mixed by an internal mixer or an open mill, uniformly mixing, and then discharging. The vulcanizing agent is mainly sulfur, the melting point of industrial sulfur is 112.8 ℃, the flash point is 207 ℃, the flash point of sulfur is basically not reached in ordinary rubber processing, and the processing safety can be ensured by controlling static electricity, open fire and the like during processing. The addition of sulfur can reduce the Mooney viscosity of the rubber compound, and the higher mixing temperature can also reduce the Mooney viscosity of the rubber compound and improve the processability.
The traditional final mixing method is to carry out final mixing on an open mill: and (3) putting the internally mixed masterbatch on an open mill, and then independently putting a vulcanizing agent and an accelerator on the open mill for adding. For example: chinese patent 202010023407.1 discloses a final mixing series homogenizing rubber mixing process, which comprises the following steps: (1) performing low-speed low-temperature final refining on the rubber material and the compounding agent at a rotating speed of not higher than 30 revolutions per minute and a rubber discharge temperature of not higher than 110 ℃; (2) cooling and tabletting the finally refined rubber material; (3) homogenizing and mixing the cooled and tabletted rubber material at low temperature; (4) tabletting and collecting the rubber material after low-temperature homogenization and mixing to obtain the rubber material; the low-temperature homogenizing and mixing in the step (3) comprises a plurality of procedures, wherein the roll spacing, the width of the rubber blocking plate, the accumulated rubber proportion, the speed of the roller and the rubber smashing time of the procedures are as follows: a first procedure: the roller spacing is 0.8mm-1.5mm, the width of the rubber baffle plate is 1.0m-2.1m, the accumulation rubber accounts for 15% -30%, the roller speed is 30m/min-50m/min, and the rubber smashing time is 20s-50 s; and a second procedure: the roller spacing is 8.0mm-10.0mm, the width of the rubber blocking plate is 1.5m-2.1m, the accumulation rubber accounts for 5% -15%, the roller speed is 20m/min-50m/min, and the rubber smashing time is 100s-400 s; the mixing process for producing final rubber compound by using a large-capacity internal mixer disclosed in Chinese patent 201610726279.0 comprises the following steps: (1) pressing a top plug, feeding and mixing for 30 seconds, wherein the pressure is 5.5bar, and a high rotating speed of 35rpm is used to generate a large shearing force, so that the rubber material can flow fast in a mixing chamber, and the feeding process is accelerated; (2) lifting the top plug, pressing the top plug, mixing for 20-30 seconds at 5.5bar, and using a medium-high rotating speed of 30rpm, wherein the flowing speed of the rubber material is high, so that the mixing and dispersion of the medicine and the rubber material are accelerated; the medicine is a vulcanizing agent and an accelerant; (3) lifting the top plug, pressing the top plug, mixing for 15-20 seconds at 5.5bar, and controlling the temperature to rise at a rotation speed of 25rpm to disperse the medicine; (4) and in the later stage of mixing, the ram is pressed after being lifted, mixing is carried out for 15 seconds at the pressure of 4.5bar, the low rotating speed of 20rpm is used, the temperature rise is slower, the mixing time is ensured, the mixing is sufficient, the medicines are uniformly dispersed, and the rubber material is uniformly mixed. However, when the final mixing mode is used, powdered sulfur can permeate into the air, so that the safety hazard is high, the final mixing efficiency of the open mill is low, and the technical requirement on operators is high. At present, the final rubber compound is processed mostly by adopting a two-section type mixing operation mode: the first stage of mixing is carried out without adding a vulcanizing agent and an accelerator, and the second stage of mixing is carried out with a vulcanizing agent and an accelerator. In order to prevent the rubber compound from scorching or blooming, the temperature during mixing is generally controlled below 110 ℃. Most of the final mixing internal mixers adopt low rotating speed to prevent temperature rise from being fast, but the shearing and kneading action of the internal mixer rotor still can generate larger temperature rise, and the primarily mixed rubber material can generate more shearing and chain breakage to influence the performance of the rubber material. Meanwhile, the rapid temperature rise can also cause short mixing time of rubber materials, uneven mixing time among different batches, large difference of vulcanization curves of final rubber mixing, low production efficiency and difficulty in meeting production requirements.
In addition, when the rubber industry carries out the final mixing of the internal mixer, the final mixing temperature is reduced as much as possible to prevent scorching, and in the final mixing process, the mixed rubber with lower temperature is quickly heated under the shearing and kneading action of the rotor; when the interval time between two mixing sections is longer, the rubber compound can be hardened, and if the hardened rubber compound is directly added during the final mixing of the internal mixer, the internal mixer can generate larger impact, so that the torque mutation is larger, the equipment is lost, and the energy consumption is increased. If the rubber compound is heated, tabletted or crushed and then added into an internal mixer, the steps are complex and the energy consumption is high.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and develops and designs a rubber final mixing process for an internal mixer, so that the final mixing time and energy consumption are reduced, the impact on equipment is reduced, and the production efficiency is improved.
In order to realize the purpose, the rubber final mixing process for the internal mixer comprises the following specific steps:
(1) raising the temperature of the mixing chamber to 120 ℃ for later use;
setting the final mixing temperature at 120 ℃ based on the characteristics of sulfur melting at 120 ℃ and the characteristics of reduction of Mooney viscosity at high temperature of the rubber compound;
(2) adding a vulcanizing agent into an internal mixing chamber at a rotating speed of below 10rpm, dropping a top plug, and preserving heat to ensure that the vulcanizing agent is completely converted into a molten state;
(3) feeding the chopped mixing rubber blocks into an internal mixing chamber at a speed of more than 50rpm, wherein the feeding speed ensures that the internal mixer has stable feeding;
(4) immediately adding an accelerant after the mixing rubber block is added, and dropping a top plug for mixing;
based on the characteristic that the Mooney viscosity of the rubber material can be reduced by adding the sulfur, the sulfur is added firstly during the final mixing, and then the accelerator is added, so that the torque during the mixing is reduced, the sulfur dispersibility is improved, and the scorching is avoided to the greatest extent.
The heat preservation time related to the step (2) is selected according to the environmental temperature and the size of the internal mixer, so that the vulcanizing agent is ensured to be fully melted; and (4) selecting the mixing time in the step (4) according to the volume and the mixing degree of the internal mixer, and ensuring full mixing.
When the rubber final mixing process for the internal mixer is used for continuous production, the temperature of an internal mixing chamber of a subsequent train is higher than 120 ℃, the melting speed of sulfur is higher, and the melting time of sulfur is adjusted according to actual conditions.
Compared with the prior art, the temperature of the mixing chamber is set to be higher, the Mooney viscosity of the rubber material is rapidly reduced under the action of liquid sulfur, the shearing action of a rotor is reduced, meanwhile, the temperature of the whole mixing chamber is reduced by the mixed rubber at a lower temperature, the temperature is kept within a proper range, the vulcanizing agent is firstly added for melting, then the mixed rubber is put into the mixing chamber, the mixed rubber is mixed uniformly by the vulcanizing agent in the heating and plastication process, the accelerating agent is added for mixing immediately after the rubber is put into the mixing chamber, the vulcanizing agent and the accelerating agent are added separately, and the accelerating agent is arranged to be added at the last, so that the scorching phenomenon of the rubber material can be avoided to the maximum extent; the principle is scientific and reliable, and the Mooney viscosity of the rubber compound is rapidly reduced due to the high temperature and the vulcanizing agent added in advance, so that the processability is improved, the impact on equipment is reduced, the energy consumption of final refining is reduced, and various properties of the vulcanized rubber are improved.
Description of the drawings:
FIG. 1 is a schematic torque comparison of two processes involved in the present invention.
The specific implementation mode is as follows:
the invention is further illustrated by the following examples in conjunction with the accompanying drawings.
Example 1:
the rubber final mixing process for the internal mixer comprises the following specific steps:
(1) raising the temperature of an internal mixing chamber with the capacity of 200mL of an RM-200C internal mixer (adopting a double-edge Benbury rotor) of Harbin electric technology Limited liability company to 120 ℃ for later use;
(2) adding sulfur into the banburying chamber at the rotating speed of 10rpm, dropping a top plug, and preserving heat for 30s to ensure that the sulfur is completely converted into a molten state; when the sulfur is added, the sulfur is prevented from falling onto the rotor, the sulfur is allowed to fall onto the wall of the mixing chamber as much as possible, the rotor and the rubber material are prevented from slipping, the friction coefficient between the wall of the mixing chamber and the rubber material is reduced, and the feeding speed is increased; the open fire and static electricity are avoided, and the high rotating speed is not used before the sulfur is melted so as to prevent the safety problem caused by the static electricity;
(3) putting the chopped mixed rubber blocks into an internal mixing chamber at the rotating speed of 50rpm, pressing a top bolt, and lifting the top bolt; the glue is likely to have the phenomenon of reverse glue when being thrown, the top bolt is fallen down to press down the glue material, and then the glue is continuously thrown;
(4) immediately adding an accelerant after the rubber feeding is finished, pressing a top bolt, mixing for 30s, and then discharging rubber; the top plug can be pressed first and then the accelerant is added, because the sulfur is uniformly distributed in the glue adding process, the accelerant is only required to be uniformly dispersed, the viscosity of the glue material is low, the processing is easy, the speed of adding the accelerant can be slightly slower, and the phenomenon of agglomeration of massive accelerant is avoided.
As a control group, a rubber finishing process for a conventional internal mixer was used: and (3) putting the rubber compound at the temperature of 70 ℃ in an internal mixing chamber at the rotating speed of 30rpm, pressing a top bolt at the rotating speed of 50rpm, lifting the top bolt, adding a vulcanizing machine and an accelerator, pressing the top bolt, mixing for 30s, and discharging the rubber.
Tread rubber formula 1(100 parts by mass of natural rubber, 53.5 parts by mass of carbon black N234, 2 parts by mass of stearic acid, 3.5 parts by mass of zinc oxide, 1.5 parts by mass of antioxidant 4020, 1 part by mass of sulfur and 1.5 parts by mass of accelerator NS) and formula 2(100 parts by mass of natural rubber, 50 parts by mass of white carbon black, 10 parts by mass of Si69, 2 parts by mass of stearic acid, 2 parts by mass of zinc oxide, 2 parts by mass of antioxidant 4020, 1.3 parts by mass of accelerator DPG, 1 part by mass of sulfur and 1.2 parts by mass of accelerator CZ) were subjected to final refining according to the processes of the examples and the control group, respectively.
The vulcanization characteristic, the physical and mechanical properties, the rubber material uniformity, the carbon black dispersion degree, the energy consumption and the torque are respectively compared and researched, and the influence of two different final refining processes on the rubber material performance is obtained:
(1) analysis of vulcanization characteristics
The test compound cure characteristics measured with a rotorless cure meter are shown in the table below:
Figure BDA0003055497120000041
Figure BDA0003055497120000051
it can be known that the final refining process of the embodiment does not have great influence on the vulcanization characteristic of the rubber compound, and for the formula 1, the final refining process of the embodiment prolongs T10, shortens T90, ensures the processing safety and improves the vulcanization efficiency; for formulation 2, the final process of the examples also had little effect on the cure characteristics. Therefore, the sulfur and the accelerator are added separately, so that the rubber material can be effectively prevented from scorching at high temperature, and the pure sulfur vulcanization efficiency is extremely low without the accelerator, so that the influence generated in the final refining process can be ignored.
(2) Physical and mechanical properties and sizing homogeneity analysis
The rubber uniformity is analyzed by a mathematical method, 10 samples are respectively made on two rubbers for testing, the standard deviation of each physical and mechanical property data of the rubber is calculated, the dispersion is measured, and the smaller the standard deviation of the properties is, the better the rubber uniformity is. Physical properties and data discrete comparative structures are shown in the following table:
Figure BDA0003055497120000052
it can be seen that, compared with the final mixing process of the control group, the final mixing process of the embodiment improves various performances of the rubber material and the uniformity of the final mixed rubber within the same time to different degrees, and the standard deviation of the performance values is smaller than that of the final mixing process of the control group.
(3) Carbon Black Dispersion analysis
The carbon black dispersity of the rubber compound in the formula 1 is tested by using a carbon black dispersity instrument, the comparison group is 6.1, the embodiment is 6.6, and in the final refining process of the embodiment, as sulfur is added earlier and is in a molten liquid state, the sulfur has the effect similar to that of operating oil, the further dispersion of the carbon black is promoted, the dispersity and the reinforcement effect of the carbon black are improved, and the physical and mechanical properties of the rubber compound can be further improved.
(4) Torque and energy consumption analysis
The energy consumption in the mixing process is calculated by using the self-contained driving software of the Harpag RM-200C, the torque data in the mixing process is derived, the torques of the two processes are drawn by origin (function drawing software), as shown in figure 1, the torque curve of the comparison group is on the whole in the embodiment, the torque mutation is large, and the impact on equipment is large.
In the final refining of the embodiment, the Mooney viscosity of the rubber material is reduced due to the action of high temperature and molten sulfur, the processability is good, the overall torque is low, and the torque fluctuation is smooth.
The energy consumption of a comparison group obtained by using a Hewlett packard internal mixer with driving software is 64kJ, the energy consumption of the embodiment is 42kJ, and the energy consumption is saved by 34 percent, because the Mooney viscosity of rubber can be reduced by high temperature and sulfur, the processing performance is improved, the impact on equipment caused by overlarge torque mutation is prevented, and the torque is also reduced.
In addition, the melting process of the sulfur can be shortened to about 10s, in the embodiment, in order to ensure that the sulfur is completely melted, the heating time is set to 30s, the heating time can be reduced as appropriate in actual production and use, and the final refining efficiency is improved.

Claims (7)

1. A rubber final refining process for an internal mixer is characterized by comprising the following specific steps:
(1) raising the temperature of the mixing chamber to 120 ℃ for later use;
(2) adding a vulcanizing agent into an internal mixing chamber, dropping a top plug, and preserving heat to ensure that the vulcanizing agent is completely converted into a molten state;
(3) putting the chopped mixing rubber blocks into an internal mixing chamber;
(4) and immediately adding the accelerator after the mixing rubber block is added, and dropping the top plug for mixing.
2. The process of claim 1, wherein in step (2), the vulcanizing agent is added to the mixing chamber at a speed of less than 10 rpm.
3. A rubber finishing process for an internal mixer according to claim 1, wherein the chopped mass of rubber in step (3) is fed into the mixing chamber at a speed of 50rpm or more.
4. A rubber finishing process for an internal mixer according to claim 1 or 3, wherein the feeding speed of the rubber mass in the step (3) is such that the internal mixer can keep stable feeding.
5. A rubber finishing process for an internal mixer according to claim 1, wherein the feeding sequence in step (4) is replaced by dropping a ram and then feeding the accelerator.
6. A rubber finishing process for an internal mixer according to claim 1 or 2, wherein the holding time in step (2) is selected according to the ambient temperature and the size of the internal mixer.
7. A rubber finishing process for an internal mixer according to claim 1 or 5, wherein the mixing time in the step (4) is selected in accordance with the volume of the internal mixer and the mixing degree.
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JP2013018212A (en) * 2011-07-12 2013-01-31 Toyo Tire & Rubber Co Ltd Apparatus for processing rubber compounded composition and processing method therefor
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CN101508811A (en) * 2009-03-10 2009-08-19 叶孙勇 Injectable vulcanizable vinyl benzene rubber particles and producing process
CN102069534A (en) * 2010-12-13 2011-05-25 青岛开世密封工业有限公司 Open mill charging method
JP2013018212A (en) * 2011-07-12 2013-01-31 Toyo Tire & Rubber Co Ltd Apparatus for processing rubber compounded composition and processing method therefor
CN105837882A (en) * 2016-05-17 2016-08-10 江苏通用科技股份有限公司 Pre-sulfurized steel wire ring steel wire isolation rubber and preparation method
CN110722703A (en) * 2019-10-23 2020-01-24 青岛科技大学 Low-temperature continuous mixing production method for rubber

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