CN114634676B - Ethylene propylene rubber wiper strip and preparation method thereof - Google Patents
Ethylene propylene rubber wiper strip and preparation method thereof Download PDFInfo
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- CN114634676B CN114634676B CN202210473521.3A CN202210473521A CN114634676B CN 114634676 B CN114634676 B CN 114634676B CN 202210473521 A CN202210473521 A CN 202210473521A CN 114634676 B CN114634676 B CN 114634676B
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
- B29B7/005—Methods for mixing in batches
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
- B29C69/02—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore of moulding techniques only
-
- 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
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
Abstract
The invention belongs to the technical field of wiper rubber, and particularly relates to an ethylene propylene rubber wiper strip and a preparation method thereof. The wiper strip is manufactured through the steps of raw material mixing, feeding, rubber discharging, rubber sheet mixing, rubber strip prefabrication and die pressing. Therefore, the invention simultaneously and greatly reduces the permanent tension deformation and the permanent compression deformation, and after the wiper strip is used for a period of time, the permanent deformation resistance of the wiper strip is strong, the recovery capability after compression/tension is strong, and the service life is also obviously prolonged.
Description
Technical Field
The invention belongs to the technical field of wiper rubber, and particularly relates to an ethylene propylene rubber wiper strip.
Background
When the windscreen wiper of the automobile is started, the driving device controls the windscreen wiper arm to swing left and right, and the windscreen wiper blades arranged on the windscreen wiper arm remove rain, snow, dust and other foreign matters on the automobile glass, so that the visual field of a driver is ensured. Since the portion of the wiper blade in direct contact with the glass surface is a strip rubber, the portion is called a wiper rubber strip (also called a wiper strip), and the quality and performance of the wiper strip determine the wiping effect of the wiper blade.
The wiper rubber strip is generally made of Natural Rubber (NR), styrene Butadiene Rubber (SBR), polychloroprene rubber (CR), ethylene propylene rubber (EPM/EPDM), silicone rubber, and the like. The problem that its exists lies in, after using a period, under windscreen wiper arm pressure effect, when the windscreen wiper piece is the bending condition, the tensile and compression deformation volume of windscreen wiper strip is big, the anti deformability of windscreen wiper strip is less than, the resilience is poor after the deformation, can cause windscreen wiper strip inclination to change greatly, form and contrary to scraping and shovel and scrape, lead to water film thickness to increase like this on the one hand, it is dirty to scrape, water smoke appears on the glass face, make the driver can not clearly observe vehicle surrounding environment and road conditions, very easily the traffic accident appears, on the other hand, the noise is big when windscreen wiper strip deformation can cause windscreen wiper arm swing upset, bring the dysphoria sense for personnel in the car, and the deformation makes windscreen wiper strip life shorten to about 50 ten thousand times in addition, need frequent replacement.
Disclosure of Invention
The invention aims to provide an ethylene propylene rubber wiper strip with stronger deformation resistance.
In order to achieve the purpose, the invention adopts the following technical scheme: the ethylene propylene rubber wiper strip comprises the following raw materials in parts by mass: 95-105 parts of ethylene propylene rubber, 4-6 parts of zinc oxide, 0.5-1.5 parts of stearic acid, 1-3 parts of anti-aging agent, 10-70 parts of carbon black, 8-25 parts of softener, 0.5-3 parts of accelerator, 1-3 parts of vulcanizing agent, 1-2 parts of dispersing flowing agent, 1-20 parts of cerium oxide and 1-30 parts of bismuth oxide.
The inventor of the patent discovers through years of experimental study that the wiper strip is mainly stressed and stretched when in use, and the wiper strip made of rubber material has high tensile permanent deformation and compression permanent deformation (the permanent deformation refers to irreversible deformation of an object under the action of the outside, and has the tensile permanent deformation and the compression permanent deformation according to the property of applying external force). Therefore, the material has poor recovery capability and short service life. .
In order to improve the deformation resistance of rubber, a vulcanizing agent is usually added during the preparation of the rubber to improve the crosslinking density of the rubber, but the inventor adopts the rubber as a wiper strip, finds that the use effect is not good, and cannot solve the problem of high permanent deformation of the wiper strip. The inventors found that the reason why the problems could not be solved with the vulcanizing agent was: the addition of the vulcanizing agent has a limitation, the addition amount of the vulcanizing agent has a certain upper limit (for example, 100 parts by mass of ethylene propylene rubber, and 1-3 parts by mass of the vulcanizing agent), and when the addition amount exceeds 3 parts, the tensile permanent deformation and the compression permanent deformation of the rubber are not reduced, namely, the improvement of the deformation resistance of the rubber is limited, and the continuous addition of the vulcanizing agent can cause excessive substances in the rubber to be sprayed on the surface to form a heterochromatic state, so that the performance of the rubber is reduced.
Therefore, through intensive research and experiments, the inventor finds a solution for improving the upper limit of the deformation resistance of the rubber, namely adding bismuth oxide and cerium oxide into the formula of the wiper strip at the same time.
Cerium oxide generally improves the heat resistance of rubber and has stronger resistance to thermal oxidation aging of rubber, and bismuth oxide generally replaces lead to be compounded with rubber so as to improve the protection performance of the rubber to X rays. The inventor further finds that the two substances have the function of enhancing the bonding force of rubber molecular chains: bismuth oxide belongs to metal oxide, has the characteristics of large specific surface area and high activity, can play a role in improving the crosslinking density in rubber, and enables the bonding force of rubber molecular chains after vulcanization to be stronger. The cerium oxide is used as a rare earth element, the stability is good, on one hand, the cerium oxide has good wettability in rubber, large interaction force with a rubber matrix, strong binding force and good interface binding, inorganic particles such as rigid chains generally play a role in enhancing the rubber, on the other hand, the reinforcing effect of the rare earth is related to a large number of f orbitals contained in the rare earth element, the special structure of the rare earth element is easy to form a complex, and the 'instantaneous crosslinking density' of the rubber is increased during stretching, so that the tensile strength of the rubber is rapidly enhanced.
However, the cerium oxide or the bismuth oxide is added separately, the bonding position of the cerium oxide or the bismuth oxide and an ethylene propylene rubber matrix is single, molecular chains of the cerium oxide or the bismuth oxide can only form a single network structure, a composite network structure cannot be formed, and the tensile permanent deformation and the compression permanent deformation cannot be reduced simultaneously. When the wiper rubber strip is used, the wiper rubber strip can simultaneously encounter stretching deformation and compression deformation, so that the two deformations are required to be reduced simultaneously, otherwise, the tensile deformation capability of the wiper rubber strip is still weaker when the wiper rubber strip is made into the wiper strip, and the problem provided by the invention cannot be solved.
Therefore, the two substances are added simultaneously, the two substances are combined with different molecular chain groups of the ethylene propylene rubber, the molecular chains are mutually crossed, a composite network structure can be formed, the bonding force on the molecular chain layer reaches an extremely high level, the material performance is reflected, the tension permanent deformation and the compression permanent deformation are simultaneously and greatly reduced, after the wiper strip is used for a period of time, the permanent deformation resistance of the wiper strip is strong, the recovery capability after compression/tension is strong, and the service life of the wiper strip is prolonged to about 130 ten thousand times from the previous 50 ten thousand times.
Furthermore, the anti-aging agent is 2, 4-trimethyl-1, 2 dihydroquinoline polymer, has excellent heat-oxygen aging resistance and can increase the heat resistance of rubber.
Furthermore, the softening agent is paraffin oil, which can increase the plasticity of the rubber compound and reduce the viscosity.
Further, the accelerator is TAIC, and can accelerate the vulcanization speed of the vulcanizing agent at the time of vulcanization.
Further, the dispersion flow agent is DEOFLOW A, so that the dispersibility of the filler is improved.
Furthermore, the vulcanizing agent is BIBP, the vulcanizing time of the organic peroxide is short, and the heat resistance of vulcanized rubber is good.
Further, 1 part of cerium oxide and 30 parts of bismuth oxide; or 20 parts of cerium oxide and 1 part of bismuth oxide; or 10 parts of cerium oxide and 15 parts of bismuth oxide.
The invention also provides a preparation method of the ethylene propylene rubber wiper strip, which comprises the following steps:
1) Preparing materials: preparing 95-105 parts of ethylene propylene rubber, 4-6 parts of zinc oxide, 0.5-1.5 parts of stearic acid, 1-3 parts of anti-aging agent, 10-70 parts of carbon black, 8-25 parts of softener, 0.5-3 parts of accelerator, 1-3 parts of vulcanizing agent, 1-2 parts of dispersing flowing agent, 1-20 parts of cerium oxide and 1-30 parts of bismuth oxide.
2) Mixing: putting ethylene propylene rubber into an enclosed rubber mixing mill, heating to 40-50 ℃, simultaneously adding zinc oxide, stearic acid, an anti-aging agent, cerium oxide and bismuth oxide, mixing and stirring for 3-4 minutes until the ethylene propylene rubber is in a viscous state;
3) Feeding: continuously heating the closed rubber mixing mill to 65-75 ℃, adding carbon black, a softening agent and a dispersing flow agent, and mixing for 4-5 minutes;
4) Rubber discharging: when the internal rubber mixing mill is continuously heated to 140-150 ℃, discharging the mixed rubber material in a viscous flow state from the internal rubber mixing mill, cooling to be less than or equal to 50 ℃, rolling the mixed rubber material into a rubber sheet with the thickness of 4-5 mm by using an open rubber mixing mill, and standing at 0-35 ℃ for more than 16 hours to diffuse molecules among different substances;
5) Mixing films: placing the rubber sheet into a closed rubber mixing mill, adding an accelerator and a vulcanizing agent at 50-60 ℃, mixing for 4-5 minutes, discharging rubber after the temperature reaches 85-95 ℃, then rolling the mixed rubber material into the rubber sheet with the thickness of 4-5 mm by using an open rubber mixing mill, and standing the rubber sheet at 0-35 ℃ for more than 16 hours to ensure that molecules among different substances are diffused;
6) Prefabricating an adhesive tape: placing the rubber sheet into a rubber preforming machine, heating to 80-120 ℃, and then forming through a mouth mold of the rubber preforming machine to prepare a standard rubber strip;
7) Rubber strip compression molding: and (3) putting the standard adhesive tape into a wiper strip mold of a flat vulcanizing machine, heating and vulcanizing at 180-200 ℃ for 5-12 minutes, and discharging after finishing.
The preparation method adopts a segmented preparation process, so that the temperature of the rubber compound in the banburying chamber is easy to control, molecules are diffused through parking when the rubber sheet is prepared, the cross-linking effect of the raw materials is improved, and the quality stability and the uniformity of the rubber compound can be ensured.
Detailed Description
The present invention will now be described by way of non-limiting examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
1. Ingredients
The following ingredients were used to prepare the raw materials for the ethylene propylene rubber wiper strips of examples 1,2 and 3, control 1 (only bismuth oxide was added), control 2 (only cerium oxide was added) and control 3 (no cerium oxide and no bismuth oxide were added), and the ingredients were as follows:
the compound raw material names corresponding to the compound raw material abbreviations in the ingredient tables are as follows:
DEOFLOW A: fatty alcohol ester joint lubricant
TAIC: triallylisocyanurate
BIBP: odorless DCP or crosslinking agent BIBP
2. Equipment preparation
Preparing and debugging a closed rubber mixing mill, an open rubber mixing mill, a rubber pre-forming machine and a flat vulcanizing machine.
3. Preparation of wiper strip
(first) wiper strips of preparation examples 1,2, 3
According to the mixture ratio of the examples 1,2 and 3 in the ingredient table, the wiper strips of the examples 1,2 and 3 are respectively prepared according to the following steps.
1. Mixing: putting ethylene propylene rubber into an enclosed rubber mixing mill, heating to 40-50 ℃, simultaneously adding zinc oxide, stearic acid, 2, 4-trimethyl-1, 2 dihydroquinoline polymer, cerium oxide and bismuth oxide, mixing and stirring for 3-4 minutes until the ethylene propylene rubber is in a viscous state;
2. feeding: continuously heating the closed rubber mixing mill to 65-75 ℃, adding carbon black, paraffin oil and DEOFLOW A, and mixing for 4-5 minutes;
3. rubber discharging: continuously heating the closed rubber mixing mill to 140-150 ℃, discharging the mixed rubber material in a viscous flow state from the closed rubber mixing mill, cooling to be less than or equal to 50 ℃, rolling the mixed rubber material into a rubber sheet with the thickness of 4-5 mm by using an open rubber mixing mill, and standing for more than 16 hours to diffuse molecules among different substances;
4. mixing films: placing the rubber sheet into a closed rubber mixing mill, adding TAIC and BIBP at 50-60 ℃, mixing for 4-5 minutes, discharging rubber after 85-95 ℃, rolling the mixed rubber material into a rubber sheet with the thickness of 4-5 mm by using an open rubber mixing mill, and standing the rubber sheet for more than 16 hours;
5. prefabricating an adhesive tape: placing the rubber sheet into a rubber preforming machine, heating to 80-120 ℃, and then forming through a mouth mold of the rubber preforming machine to prepare a standard rubber strip;
6. rubber strip compression molding: and (3) putting the standard adhesive tape into a wiper strip mold of a flat vulcanizing machine, heating and vulcanizing at 180-200 ℃ for 5-12 minutes, and discharging after finishing so as to prepare the wiper strip.
The viscous flow state is a special term of polymer physical rheology, and refers to the mechanical state of amorphous polymer under the action of high temperature and large external force for a long time.
(II) wiper strip for preparing comparison group 1
The raw materials were prepared according to the formulation of control 1 in the formulation table, and the preparation method was the same as in examples 1,2, and 3, except that only bismuth oxide and no cerium oxide were added.
(III) wiper strip for preparing comparison group 2
The raw materials were prepared according to the formulation of control group 2 in the formulation table, and the preparation method was the same as in examples 1,2, and 3, except that only cerium oxide was added and bismuth oxide was not added.
(IV) wiper strip for preparing comparison group 3
The raw materials were prepared according to the formulation of control group 3 in the formulation table, and the preparation method was the same as in examples 1,2, and 3, except that no cerium oxide or cerium oxide was added.
4. Wiper strip performance test
The compression set and the tensile set of the wiper strips of 6 groups in total were measured in examples 1 to 3 and comparative groups 1 to 3, and the measurement methods were as follows:
(1) Compression set test: according to the standard requirements of GB/T7759.1-2015 vulcanized rubber or thermoplastic rubber compression set determination part 1, under normal temperature and high temperature conditions, wiper strip samples with diameters of 29mm +/-0.5 mm and heights of 12.5mm +/-0.5 mm are prepared, the compression ratio is 25%, and the test is carried out at the specified temperature (90 ℃ multiplied by 22 h).
(2) Tensile set test: according to the standard requirement of GB/T528-2009 vulcanized rubber or thermoplastic rubber tensile stress strain performance measurement, 3 wiper strip samples with the length of 10cm are taken, two marked lines with the distance of 5cm are drawn, the samples are clamped on a clamp and stretched by 50%, and the samples are installed for 15min and then placed in a 90 ℃ oven for 48h. After the test, the tensile state was maintained and the temperature was returned to room temperature, and the test was relaxed. The measurements were taken 30min after relaxation.
The test results were as follows:
| test items | Example 1 | Example 2 | Example 3 | Control group 1 | Control group 2 | Control group 3 |
| Compression set (%) | 10.3 | 9.2 | 6.3 | 12.7 | 11.4 | 16.7 |
| Tensile set (%) | 11.2 | 11.6 | 7.6 | 12.8 | 12.4 | 15.4 |
The test result shows that:
compression set (one):
the samples of example 1, example 2, and example 3 had compression set much less than the samples of control 1, control 2, and control 3:
(1) Compared with the single addition of cerium oxide or bismuth oxide: the highest value of example 1 in examples 1 to 3 and the lowest value of control group 2 in control groups 1 and 2, so that the compression set of example 1 is reduced by 9% (calculated by (11.4-10.3)/11.4) compared with example 1 and control group 2, that is, the compression set can be reduced by 9% by adding cerium oxide and bismuth oxide at the same time in the test, and the reduction is very obvious.
(2) Compared with no addition of cerium oxide or bismuth oxide: compared with the control group 3, the reduction of 38 percent (according to (16.7-10.3)/16.7) is higher in the example 1.
(II) permanent tensile set
The rubber samples of example 1, example 2, and example 3 had much less tensile set than control 1, control 2, and control:
(1) Compared with the single addition of cerium oxide or bismuth oxide: the highest value was found in example 2 of examples 1 to 3, and the lowest value was found in control group 2 of control groups 1 and 2. Thus, compared with example 2 and control group 2, example 2 is reduced by 6% (calculated according to (12.4-11.6)/12.4), and the reduction is very obvious.
(2) Compared with no addition of cerium oxide or bismuth oxide: compared with example 2 and control group 3, example 2 has a 24 percent (calculated according to (15.4-11.6)/15.4) reduction, and the reduction is higher.
In summary, the embodiments 1,2, and 3 of the present invention have significant effects in reducing the compression set and the tension set of the wiper rubber strip, and can effectively improve the permanent deformation resistance of the wiper strip.
The above description is only an example of the present invention, and the general knowledge of the known specific technical solutions and/or characteristics and the like in the solutions is not described herein too much. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (7)
1. The ethylene propylene rubber wiper strip is characterized by comprising the following raw materials in parts by mass: 95-105 parts of ethylene propylene rubber, 4-6 parts of zinc oxide, 0.5-1.5 parts of stearic acid, 1-3 parts of anti-aging agent, 10-70 parts of carbon black, 8-25 parts of softener, 0.5-3 parts of accelerator, 1-3 parts of vulcanizing agent, 1-2 parts of dispersing flowing agent, cerium oxide and bismuth oxide; 1 part of cerium oxide and 30 parts of bismuth oxide; or 20 parts of cerium oxide and 1 part of bismuth oxide; or 10 parts of cerium oxide and 15 parts of bismuth oxide.
2. The ethylene propylene rubber wiper strip according to claim 1, wherein: the anti-aging agent is 2, 4-trimethyl-1, 2 dihydroquinoline polymer.
3. The ethylene propylene rubber wiper strip according to claim 2, wherein: the softening agent is paraffin oil.
4. The ethylene propylene rubber wiper strip according to claim 3, wherein: the accelerator is TAIC.
5. The ethylene propylene rubber wiper strip according to claim 4, wherein: the vulcanizing agent is BIBP.
6. The ethylene propylene rubber wiper strip according to claim 5, wherein: the dispersion flow agent is DEOFLOW A.
7. The preparation method of the ethylene propylene rubber wiper strip is characterized by comprising the following steps:
1) Preparing materials: preparing each of the raw materials of claim 1;
2) Mixing: putting the ethylene propylene rubber into an enclosed rubber mixing mill, heating to 40-50 ℃, simultaneously adding zinc oxide, stearic acid, an anti-aging agent, cerium oxide and bismuth oxide, mixing and stirring for 3-4 minutes until the ethylene propylene rubber is in a viscous state;
3) Feeding: continuously heating the closed rubber mixing mill to 65-75 ℃, adding carbon black, a softening agent and a dispersing flow agent, and mixing for 4-5 minutes;
4) Rubber discharging: when the internal rubber mixing mill is continuously heated to 140-150 ℃, discharging the mixed rubber material in a viscous flow state from the internal rubber mixing mill, cooling to be less than or equal to 50 ℃, rolling the mixed rubber material into rubber sheets with the thickness of 4-5 mm by using an open rubber mixing mill, and standing for more than 16 hours at the temperature of 0-35 ℃;
5) Mixing films: putting the rubber sheet into an internal rubber mixing mill, adding an accelerant and a vulcanizing agent at 50-60 ℃, mixing for 4-5 minutes, discharging rubber after the temperature reaches 85-95 ℃, rolling the mixed rubber material into rubber sheets with the thickness of 4-5 mm by using an open rubber mixing mill, and standing for more than 16 hours at 0-35 ℃;
6) Prefabricating an adhesive tape: placing the rubber sheet into a rubber preforming machine, heating to 80-120 ℃, and then forming through a mouth mold of the rubber preforming machine to prepare a standard rubber strip;
7) Rubber strip compression molding: and (3) putting the standard rubber strip into a wiper strip mold of a flat vulcanizing machine, heating and vulcanizing at 180-200 ℃ for 5-12 minutes, and discharging after finishing vulcanization.
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