CN112778585B - Positioning node rubber composition and preparation method thereof - Google Patents
Positioning node rubber composition and preparation method thereof Download PDFInfo
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- CN112778585B CN112778585B CN202011615301.7A CN202011615301A CN112778585B CN 112778585 B CN112778585 B CN 112778585B CN 202011615301 A CN202011615301 A CN 202011615301A CN 112778585 B CN112778585 B CN 112778585B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
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- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
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Abstract
The invention provides a positioning node rubber composition which comprises the following components in parts by weight: 40-60 parts of chloroprene rubber; 20-30 parts of isoprene rubber; 10-30 parts of epoxy natural rubber; 3-5 parts of Arabic gum; 1.5-3 parts of stearic acid; 0.5-2 parts of polyethylene glycol; 3-9 parts of an anti-aging agent; 1-3 parts of microcrystalline wax; carbon black N3305-10 parts; 5-15 parts of nano-scale silicon dioxide; 5-10 parts of unsaturated carboxylic acid; 5-15 parts of zinc oxide; 1-3 parts of magnesium oxide; 0.3-1 part of sulfur; 0.5-1.7 parts of an accelerator; 1-2 parts of DCP; 3-5 parts of calcium oxide, aiming at providing an insulating rubber composition which can simultaneously meet the two technical requirements of more than 32h of cracking occurrence in a dynamic ozone test of 50pphm multiplied by 40 ℃ multiplied by 0-20 percent and less than-50 ℃ of low-temperature embrittlement temperature.
Description
Technical Field
The invention belongs to the technical field of rubber, and particularly relates to a positioning node rubber composition and a preparation method thereof.
Background
A series of positioning nodes can restrict the mutual positions of the wheel set and the framework, so that the position of the axle box on the bogie and the movement range are limited within a certain range, the load is transmitted and distributed to the wheel set, the wheel set can rotate flexibly, and the bogie can smoothly pass through a curve. A series of positioning nodes are composed of a mandrel and elastic rubber and serve as a motor train type A component, once the rubber performance cannot meet the requirement, problems occur in the running process of a train, the train can be unstable and even derailed, and therefore the rubber formula of the positioning nodes is of great importance.
According to the technical requirements of hardness and tensile strength of products and the application of the rubber as a damping part in practical use, the traditional rubber is natural rubber and chloroprene rubber. Natural rubber has good low temperature resistance but poor ozone resistance, and even if a large amount of an antioxidant is added, the rubber cracks in less than 32 hours in a dynamic ozone test at 50pphm x 40 ℃ x 0-20%; chloroprene rubber has good ozone resistance but poor low-temperature resistance, and even if a large amount of plasticizer is added, the lowest low-temperature embrittlement temperature is-45 ℃; natural rubber and ethylene propylene rubber, 50pphm x 40 ℃ x 0-20% dynamic ozone test for 32 hours, no crack, but the tensile strength is less than 19.6MPa; the dynamic ozone test of 50pphm × 40 ℃. Times.0-20% of natural rubber using butadiene rubber in combination or natural rubber using a small amount of chloroprene rubber in combination revealed that the rubber cracked in less than 32 hours.
The prior art therefore remains to be improved.
Disclosure of Invention
The present invention aims to provide an insulating rubber composition which can satisfy both the technical requirements of 50pphm x 40 ℃ x 0-20% E dynamic ozone test cracking occurrence of 32 hours or more and low-temperature embrittlement temperature-50 ℃ or less.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a positioning node rubber composition comprises the following components in parts by weight: 40-60 parts of chloroprene rubber; 20-30 parts of isoprene rubber; 10-30 parts of epoxy natural rubber; 3-5 parts of Arabic gum; 1.5-3 parts of stearic acid; 0.5-2 parts of polyethylene glycol; 3-9 parts of an anti-aging agent; 1-3 parts of microcrystalline wax; carbon black N3305-10 parts; 5-15 parts of nano-scale silicon dioxide; 5-10 parts of unsaturated carboxylic acid; 5-15 parts of zinc oxide; 1-3 parts of magnesium oxide; 0.3-1 part of sulfur; 0.5-1.7 parts of an accelerator; 1-2 parts of DCP; 3-5 parts of calcium oxide;
specifically, considering that a series of positioning node products have the requirements of ozone resistance and fatigue resistance tests, the heat generation and the permanent deformation of isoprene rubber are lower than those of natural rubber, and the fatigue resistance is better; the epoxy natural rubber has low double bond content and good ozone resistance, so that the epoxy natural rubber is selected from chloroprene rubber and isoprene rubber.
The anti-aging agent is a mixture of anti-aging agent 4010NA, anti-aging agent 4020 and anti-aging agent RD, and the weight ratio of the anti-aging agent to the anti-aging agent RD is 1:1:1, mixing;
the accelerant consists of the following components in parts by weight: accelerator NA-220.1-0.3 part; 0.1-0.4 part of accelerator DM; 0.2-0.6 part of accelerator CZ; 0.1-0.4 part of accelerator TT;
the invention also provides a preparation method of the positioning node rubber composition, which comprises the following steps:
(1) Weighing: weighing the raw materials according to the proportion in the formula;
(2) Pretreatment of raw materials: uniformly mixing the carbon black N330, the nano-scale silicon dioxide and the unsaturated carboxylic acid weighed in the step (1), activating for twenty minutes by microwave, and cooling for later use;
(3) Primary pressurizing and mixing: adding chloroprene rubber, isoprene rubber, epoxy natural rubber, arabic gum, the carbon black N330 treated in the step (1), nano-silicon dioxide, unsaturated carboxylic acid and half of zinc oxide into an internal mixer for mixing, wherein the upper plug pressure is 0.5-0.6MPa, and the mixing time is 3-5 minutes;
(4) Secondary pressurizing and mixing: adding stearic acid, polyethylene glycol, an anti-aging agent, microcrystalline wax and calcium oxide into an internal mixer for mixing, wherein the top plug pressure is 0.5-0.6MPa, and the mixing time is 1-3 minutes;
(5) Thirdly, pressurizing and mixing, namely adding the magnesium oxide, the residual zinc oxide, the sulfur, the accelerant and the DCP into an internal mixer for mixing, wherein the top plug pressure is 0.5-0.6MPa, and the mixing time is 1-3 minutes;
(6) And (3) sheet discharging: and (5) discharging the rubber processed in the step (5) to an open mill, and adjusting the roll spacing to 2mm and lower the sheet.
The invention has the beneficial effects that:
1. the rubber refined by the invention can meet all rubber technical requirements of a series of positioning nodes, the hardness (Share A) is 45 +/-3 HA, the tensile strength is more than 19.6MPa, the elongation at break is more than 450%, the compression permanent deformation is less than 20% at 70 ℃ multiplied by 24 multiplied by 25%, the cracking occurs for more than 200h in a static ozone test at 50pphm multiplied by 40 ℃ multiplied by 20E, the cracking occurs for more than 32h in a dynamic ozone test at 50pphm multiplied by 40 ℃ multiplied by 0-20E, the applied voltage is more than 1.0 multiplied by 108 omega in an electric insulation resistance at 500V, the low-temperature embrittlement temperature is less than-50 ℃, the thermal aging hardness change point is less than 7 at 70 ℃ multiplied by 96h, the tensile strength changes less than 15%, the elongation at break changes less than 20%, the fatigue test of the product can reach more than 600 ten thousand times, compared with other similar products, the rubber HAs better elasticity, good vibration damping effect, smaller dynamic stiffness/static stiffness, smaller intramolecular friction, lower internal consumption, better fatigue test effect and longer service life.
2. According to the invention, unsaturated carboxylic acid, zinc oxide and magnesium oxide are added, a neutralization reaction is carried out in the mixing and shearing process to generate MSUCA monomer particles in situ, MSUCA is grafted to a rubber molecular chain by DCP in the vulcanization process to form a nano ion cluster and ion cross-linked bond structure, when the rubber molecular chain is acted by external stress, the ion cross-linked bond can generate recombination and mechanical relaxation phenomena similar to a polysulfide cross-linked bond, the action not only can effectively relax the external stress, but also can enable the rubber molecular chains to be more orderly arranged through relative sliding, so that the stress is commonly borne, the generation of stress concentration is avoided, the heat generation in the product fatigue process is reduced, and the fatigue resistance of the product is improved.
3. The nano-silica is added, so that the reinforcing effect is better, the conductivity of the carbon black in the rubber is reduced, and meanwhile, cations are generated by friction in the mixing process, so that the insulating property of the rubber is improved, and the insulating requirement of a product is met.
4. Compared with the traditional processing technology of small material-large material-vulcanizing agent, the processing technology of large material-small material-vulcanizing agent in the invention ensures that MSUCA generated by in-situ reaction has higher initial dispersion degree and smaller initial particle size in rubber compound, and can obtain higher in-situ polymerization conversion rate, so that rubber has higher ionic bond crosslinking density and mechanical property; compared with the traditional method of adding the sulfur accelerator to the open mill, the method of the invention adds the sulfur accelerator to the internal mixer, thereby avoiding the reduction of the mechanical property of the rubber caused by repeated remixing.
5. The calcium oxide is added and serves as an alkaline substance, so that the calcium oxide can neutralize redundant acid, provide an alkaline environment for rubber materials, promote vulcanization of rubber, improve mechanical properties of the rubber, and serve as a defoaming agent to improve density of the rubber.
6. The gum arabic is added, is a natural gum and is environment-friendly, safe and harmless; the rubber is heated to be softened at normal temperature, can absorb heat generated by rubber deformation in the product fatigue test process, and simultaneously plays a role of a plasticizer after being heated and softened, so that heat generation is reduced, and the fatigue resistance of the product is improved.
7. Before mixing, the carbon black N330, the nano-scale silicon dioxide and the unsaturated carboxylic acid are subjected to microwave activation treatment, and the unsaturated carboxylic acid can be fully and uniformly mixed with the carbon black N330 and the nano-scale silicon dioxide during activation, so that corrosion to mixing equipment is avoided; the dispersibility of the unsaturated carboxylic acid is improved, the in-situ polymerization reaction efficiency is further improved, and the ionic crosslinking density is improved, so that the fatigue resistance of the rubber is improved; the microwave activation increases the surface active groups of the nano-scale silicon dioxide, and improves the dispersibility and the reinforcing effect of the nano-scale silicon dioxide in the rubber material.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is explained below by way of specific embodiments.
Example one
The positioning node rubber composition comprises the following components in parts by weight:
40 parts of chloroprene rubber; 30 parts of isoprene rubber; 30 parts of epoxy natural rubber; 2 parts of stearic acid; 1 part of polyethylene glycol; anti-aging agent 4010NA2 parts; 40202 parts of an anti-aging agent; 2 parts of an anti-aging agent RD; 3 parts of microcrystalline wax; 5 parts of calcium oxide; 5 parts of Arabic gum; carbon black N33010 parts; 5 parts of nano-scale silicon dioxide; 10 parts of unsaturated carboxylic acid; 3 parts of magnesium oxide; 15 parts of zinc oxide; 1 part of sulfur; accelerant NA-220.1 parts; 0.4 part of accelerator DM; 0.6 part of accelerator CZ; 0.4 part of accelerator TT; 1 part of DCP;
the preparation method comprises the following steps:
(3) Weighing: weighing the raw materials according to the proportion in the formula;
(4) Pretreatment of raw materials: uniformly mixing the carbon black N330, the nano-scale silicon dioxide and the unsaturated carboxylic acid weighed in the step (1), activating for twenty minutes by microwave, and cooling for later use;
(3) Primary pressurizing and mixing: adding chloroprene rubber, isoprene rubber, epoxy natural rubber, arabic gum, the carbon black N330 treated in the step (1), nano-silicon dioxide, unsaturated carboxylic acid and 7.5 parts of zinc oxide into an internal mixer for mixing, wherein the top plug pressure is 0.5-0.6MPa, and the mixing time is 5 minutes;
(4) Secondary pressurizing and mixing: adding stearic acid, polyethylene glycol, an anti-aging agent, microcrystalline wax and calcium oxide into an internal mixer for mixing, wherein the upper plug pressure is 0.5-0.6MPa, and the mixing time is 3 minutes;
(5) Thirdly, pressurizing and mixing, namely adding the magnesium oxide, the rest 7.5 parts of zinc oxide, sulfur, the accelerant and the DCP into an internal mixer for mixing, wherein the top plug pressure is 0.5-0.6MPa, and the mixing time is 3 minutes;
(6) And (3) sheet discharging: and (6) discharging the rubber processed in the step (5) onto an open mill, and adjusting the roll spacing to 2mm and lower the sheet.
Comparative example 1
A node rubber composition was the same as in example except that 30 parts by weight of isoprene rubber and 30 parts by weight of epoxidized natural rubber were replaced with 60 parts by weight of natural rubber.
Comparative example No. two
The formula and the preparation method of the positioning node rubber composition are the same as those of the first embodiment, and only the nano-scale silicon dioxide is absent.
Comparative example No. three
The formula is consistent with the embodiment, the difference is that the preparation method of the positioning node rubber composition is different, the embodiment adopts the traditional process of small material-large material-vulcanizing agent, and the preparation method is as follows:
(1) Weighing: weighing the raw materials according to the proportion in the formula;
(2) Pretreatment of raw materials: uniformly mixing the carbon black N330, the nano-scale silicon dioxide and the unsaturated carboxylic acid weighed in the step (1), activating for twenty minutes by microwave, and cooling for later use;
(3) Primary pressurizing and mixing: chloroprene rubber, isoprene rubber, epoxy natural rubber, stearic acid, polyethylene glycol, an anti-aging agent, microcrystalline wax and calcium oxide are added into an internal mixer for mixing, the top plug pressure is 0.5-0.6MPa, and the mixing time is 5 minutes;
(4) Secondary pressurizing and mixing: adding Arabic gum, carbon black N330, nano-scale silicon dioxide, unsaturated carboxylic acid and 7.5 parts of zinc oxide into an internal mixer for mixing, wherein the upper plug pressure is 0.5-0.6MPa, and the mixing time is 3 minutes;
(5) And (3) sheet discharging: discharging the rubber material obtained in the step (3) onto an open mill, turning over the rubber material on the open mill for 4 times, then uniformly adding magnesium oxide, the rest 7.5 parts of zinc oxide, sulfur, an accelerator and DCP, turning over for 4 times, finally adjusting the roll spacing of the open mill to be 0.5mm, adjusting the roll spacing to be 2mm after 5 times of thin passing, and cooling the sheet.
Comparative example No. four
A positioning node rubber composition is as in the examples in parts by weight.
The preparation method of the positioning node rubber composition is the same as that of the first embodiment, and only the difference is that calcium oxide is absent.
Comparative example five
A positioning node rubber composition is as in the examples in parts by weight.
The preparation method of the positioning node rubber composition is the same as that of the first embodiment, and only the point that the Arabic gum is lacked is different.
Comparative example six
A positioning node rubber composition is as in the examples in parts by weight.
A method for preparing a positioning node rubber composition is the same as that of example one, except that step (2) is omitted.
The rubber materials of the embodiment 1 and the comparative examples 1 to 6 are subjected to performance test, wherein the rubber hardness is tested according to a method specified in GB/T531, and the tensile strength and the elongation at break are tested according to a method specified in GB/T528; the compression set was measured according to the method specified in GB/T7759, the ozone resistance was measured according to the method specified in GB/T7762, the electric insulation resistance was measured according to the method specified in GB/T1692, the low-temperature embrittlement temperature was measured according to the method specified in GB/T1682, and the heat aging property was measured according to the method specified in GB/T3512, and the results of the measurements are shown in Table 1.
Table 1:
from the comparison of example 1 with comparative example 1, it can be seen that 20 to 30 parts of isoprene rubber in combination with 10 to 30 parts of epoxy natural rubber and with 40 to 60 parts of chloroprene rubber are much better in dynamic ozone resistance and fatigue resistance than 40 to 60 parts of natural rubber and with 40 to 60 parts of chloroprene rubber.
By comparing example 1 with comparative example 2, it can be seen that the addition of nano-sized silica can significantly improve the tensile strength and electrical insulation properties of the rubber.
By comparing example 1 with comparative example 3, it can be seen that the processing technique employed in the present invention can significantly improve the tensile strength and fatigue resistance of the rubber compared to the conventional processing technique.
By comparing example 1 with comparative example 4, it can be seen that the addition of calcium oxide can significantly improve the tensile strength and fatigue resistance of the rubber because the addition of calcium oxide promotes vulcanization of the rubber, increasing the crosslink density of the rubber.
By comparing example 1 with comparative example 5, it can be seen that the addition of gum arabic can significantly improve the fatigue resistance of the rubber.
By comparing example 1 with comparative example 6, it can be seen that the tensile strength and fatigue resistance of the rubber can be significantly improved by subjecting carbon black N330, nano-silica, and unsaturated carboxylic acid to microwave activation.
The foregoing is only a preferred embodiment of the present invention, and it will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the principle of the invention, and such modifications and improvements are also considered to be within the scope of the invention.
Claims (3)
1. A positioning node rubber composition is characterized by comprising the following components in parts by weight: 40-60 parts of chloroprene rubber; 20-30 parts of isoprene rubber; 10-30 parts of epoxy natural glue; 3-5 parts of Arabic gum; 1.5-3 parts of stearic acid; 0.5-2 parts of polyethylene glycol; 3-9 parts of an anti-aging agent; 1-3 parts of microcrystalline wax; carbon black N3305-10 parts; 5-15 parts of nano-scale silicon dioxide; 5-10 parts of unsaturated carboxylic acid; 5-15 parts of zinc oxide; 1-3 parts of magnesium oxide; 0.3-1 part of sulfur; 0.5-1.7 parts of an accelerator; 1-2 parts of DCP; 3-5 parts of calcium oxide;
the preparation method of the positioning node rubber composition comprises the following steps:
(1) Weighing: weighing the raw materials according to the proportion in the formula;
(2) Pretreatment of raw materials: uniformly mixing the carbon black N330, the nano-scale silicon dioxide and the unsaturated carboxylic acid weighed in the step (1), activating for twenty minutes by microwave, and cooling for later use;
(3) Primary pressurizing and mixing: adding chloroprene rubber, isoprene rubber, epoxy natural rubber, arabic gum, the carbon black N330 treated in the step (1), nano-silicon dioxide, unsaturated carboxylic acid and half of zinc oxide into an internal mixer for mixing, wherein the upper plug pressure is 0.5-0.6MPa, and the mixing time is 3-5 minutes;
(4) Secondary pressurizing and mixing: adding stearic acid, polyethylene glycol, an anti-aging agent, microcrystalline wax and calcium oxide into an internal mixer for mixing, wherein the upper plug pressure is 0.5-0.6MPa, and the mixing time is 1-3 minutes;
(5) Thirdly, pressurizing and mixing, namely adding the magnesium oxide, the residual zinc oxide, the sulfur, the accelerant and the DCP into an internal mixer for mixing, wherein the top plug pressure is 0.5-0.6MPa, and the mixing time is 1-3 minutes;
(6) And (3) sheet discharging: and (6) discharging the rubber processed in the step (5) onto an open mill, and adjusting the roll spacing to 2mm and lower the sheet.
2. The positioning node rubber composition according to claim 1, wherein the anti-aging agent is a mixture of anti-aging agent 4010NA, anti-aging agent 4020 and anti-aging agent RD, and the weight ratio of the anti-aging agent to the anti-aging agent RD is 1:1:1 are mixed.
3. The positioning node rubber composition of claim 1, wherein the accelerator comprises the following components in parts by weight: accelerant NA-220.1-0.3 parts; 0.1-0.4 part of accelerator DM; 0.2-0.6 part of accelerator CZ; 0.1-0.4 part of accelerator TT.
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