CN110330750A - A kind of low compression set carboxylic acid type acrylic rubber and preparation method thereof - Google Patents

A kind of low compression set carboxylic acid type acrylic rubber and preparation method thereof Download PDF

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Publication number
CN110330750A
CN110330750A CN201910611537.4A CN201910611537A CN110330750A CN 110330750 A CN110330750 A CN 110330750A CN 201910611537 A CN201910611537 A CN 201910611537A CN 110330750 A CN110330750 A CN 110330750A
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carboxylic acid
acid type
acrylic rubber
compression set
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CN110330750B (en
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李照华
唐坤明
唐燕
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Sichuan Qinglong Acrylate Rubber Co Ltd
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Sichuan Qinglong Acrylate Rubber Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/205Compounds containing groups, e.g. carbamates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/29Compounds containing one or more carbon-to-nitrogen double bonds
    • C08K5/31Guanidine; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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Abstract

The present invention provides a kind of low compression set carboxylic acid type acrylic rubber and preparation method thereof, belongs to synthetic rubber cooperation, processing technique field.A kind of low compression set carboxylic acid type acrylic rubber, its raw material include: according to parts by weight 100 parts of carboxylic acid type acrylic rubber, it is fast extrude carbon black 10-50 part, 10-50 parts of precipitated silica, 1-5 parts, No. 1 1-3 parts of vulcanizing agent of silane coupling agent, 1-4 parts of promotor, 1-3 parts of processing aid and 2-5 parts of anti-aging agent, the mass ratio of fast extrude in carbon black and precipitated silica is 1:1.Not only there is preferable low compression set performance, while also there is preferable thermal stability, higher hardness and higher tensile strength.A kind of preparation method of low compression set carboxylic acid type acrylic rubber, silane coupling agent are added when the temperature of rubber compound is 50-70 DEG C, and method is simple, and the carboxylic acid type acrylic rubber of preparation has preferable performance.

Description

A kind of low compression set carboxylic acid type acrylic rubber and preparation method thereof
Technical field
The invention belongs to synthetic rubber cooperations, processing technique field, specifically, being related to a kind of low compression set carboxylic Acid type acrylic rubber and preparation method thereof.
Background technique
Acrylic rubber (ACM) is by acrylate and with monomer that can provide activity of cross-linking reaction group etc. through altogether An elastic-like material made of poly-, main chain is saturated structures, thus has heat-resisting, ultra-violet radiation resisting and ozone proof property Energy;Contain polar ester groups on its side chain, thus also there is excellent oil resistance.Acrylic rubber is mainly applicable to Sealing element and the oil pipe etc. for making heat-resisting oil resistant are mainly used for the neck such as automobile, motorcycle, power transformer, naval vessel, petrochemical industry Domain.
The compression set of acrylic rubber is bigger, this is the performance deficiency as sealing material, deforms great Rong It easily causes poorly sealed, is easy to produce the adverse consequences of oil leak.
The physical mechanical property of acrylic rubber is influenced by multifactor, comprising: the structure (original of polymer of rubber Material proportion), the molecular weight of rubber, the cooperation processing technology of rubber etc..
Acrylic rubber has different types, more commonly used at present to have: Active Chlorine by the type point of cure site monomer Type, carboxylic acid type, epoxy type etc., different types of acrylic rubber have different cooperation processing technologies.Different types of rubber There is different compression set performances, comparatively, the compression set performance of carboxylic acid type rubber is relatively good, better than activity Chlorine type and epoxy type rubber, but for using effect, the higher the better for compression set performance, it can satisfy some make With the requirement of condition harshness, so, the compression set performance for improving carboxylic acid type rubber still has great importance.
In the cooperation processing link of carboxylic acid type acrylic rubber, at present reduce sizing material compression set method and Effect is as follows:
1, in surface side filler, the filler of acrylic rubber is suitble to have carbon black (except acid channel carbon black), the precipitation method White carbon black (except acid fume colloidal silica), precipitated calcium carbonate etc..
White carbon black is generally required to be pre-processed with silane coupling agent, one end and the white carbon black molecular link phase chain of coupling agent It connects, other end is linked with rubber molecule key, plays " gantry ", to form the binding force of rubber and white carbon black strand.It passes The processing method of system is silane coupling agent to be directly added into white carbon black to be uniformly mixed, and makes one end and the white carbon black molecule of coupling agent Bond is closed, and other end is vacant, is waited and being closed with rubber molecule bond.
Filler influences the compression set performance of sizing material bigger.
Soft black is selected, such as LR low reinforcings such as carbon black and precipitated calcium carbonate, beautiful English powder, talcum powder by spraying is inorganic Filler can make rubber keep relatively good elasticity, these fillers have good heat aging property, thus have to reduce and compress The effect of permanent deformation.But these fillers are poor to the reinforcing effect of sizing material, influence the importance such as hardness, the tensile strength of sizing material Energy index, scope of application critical constraints.
Hard carbon black (such as: high abrasion carbon black, fast extrusion carbon black etc.) reinforcing effect is good, but the poor flexibility of sizing material, it is resistance to Heat aging performance is poor, thus the compression set of sizing material is big.
Precipitated silica heat aging property in inorganic filler is good, and reinforcing effect is good, but the poor flexibility of sizing material, because And compression set is big.
2, extend vulcanization time, reduce deformation to improve state of cure (vulcanization).
It is effective in the case where rubber vulcanization is insufficient, under the conditions of vulcanization has been compared adequately, reduce compression forever The effect deformed long is less obvious.
The generally existing some disadvantages of these methods cannot improve the hard of sizing material while reducing sizing material compression set Degree and tensile strength.
Summary of the invention
The purpose of the present invention is to provide a kind of low compression set carboxylic acid type acrylic rubber, not only have preferable Compression set performance, while also have preferable thermal stability, higher hardness and higher tensile strength.
Another object of the present invention is to provide a kind of preparation sides of low compression set carboxylic acid type acrylic rubber Method, method is simple, and the carboxylic acid type acrylic rubber of preparation has preferable comprehensive performance.
In order to achieve the above object, the solution that the present invention uses is:
A kind of low compression set carboxylic acid type acrylic rubber, raw material include: carboxylic acid type third according to parts by weight 100 parts of olefin(e) acid ester rubber, fast extrusion carbon black 10-50 parts, 1-5 parts, No. 1 10-50 parts of precipitated silica, silane coupling agent vulcanizing agent 1-3 parts, 2-6 parts of promotor, 1-3 parts of processing aid and 2-5 parts of anti-aging agent, the fast mass ratio for extruding carbon black and precipitated silica For 1:1, the mass ratio of No. 1 vulcanizing agent and promotor is 1:2.
A kind of preparation method of low compression set carboxylic acid type acrylic rubber, comprising the following steps:
By carboxylic acid type acrylic rubber, carbon black, precipitated silica, processing aid and anti-aging agent addition open mill are extruded fastly The first rubber compound is made in middle progress first time mixing;
When the temperature of the first rubber compound is 50-70 DEG C, silane coupling agent is added, is uniformly mixed, the second rubber compound is made;
Then No. 1 vulcanizing agent and promotor is added, then carries out sulfidization molding, low compression set carboxylic acid type propylene is made Acid esters rubber.
The beneficial effect of low compression set carboxylic acid type acrylic rubber provided by the invention and preparation method thereof is, Wherein, by extruding being used cooperatively for carbon black and precipitated silica fastly, while being made by the cooperation of No. 1 vulcanizing agent and promotor With, make the carboxylic acid type acrylic rubber prepared have preferable heat aging performance and low compression set performance;In glue Material adds silane coupling agent during being kneaded, carboxylic acid type acrylic rubber and white carbon black are uniformly present in system simultaneously In, when addition, the both ends of silane coupling agent can avoid silane coupling agent and pre-process white carbon black simultaneously with two objects ining conjunction with When, one end is combined, and other end is by long-term vacant situation, wherein when silane coupling agent mixing is added, the first rubber compound Temperature at 50-70 DEG C, each strand has relatively high kinetic energy, this is conducive to silane coupling agent and rubber and white carbon black strand It is quick, firm connection, the coupling intensity between rubber and white carbon black is greatly improved, so that the net formed when the vulcanization of rubber Shape structural molecule chain has better anti-pressure ability, improves the compression set performance of rubber.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase Product.
Below to a kind of low compression set carboxylic acid type acrylic rubber of the embodiment of the present invention and preparation method thereof It is specifically described.
A kind of low compression set carboxylic acid type acrylic rubber provided in an embodiment of the present invention, raw material is by weight Number meter include: 100 parts of carboxylic acid type acrylic rubber, it is fast extrude carbon black 10-50 parts, it is 10-50 parts of precipitated silica, silane coupled 1-5 parts, No. 1 1-3 parts of vulcanizing agent of agent, 2-6 parts of promotor, 1-3 parts of processing aid and 2-5 parts of anti-aging agent.It is fast extrude carbon black with The mass ratio of precipitated silica is 1:1, and the mass ratio of No. 1 vulcanizing agent and promotor is 1:2.
Wherein, the kind that carbon black is hard carbon black is extruded fastly, is produced by Audit For Process, and partial size is 40~48nm.Due to Partial size is larger, and structure is higher, can assign the good processing performance of sizing material and higher stress at definite elongation, heat is small and thermal conductivity is good It is good, but high temperature resistance is not fine.Precipitated silica due to porosity and big specific surface area, have in raw rubber compared with Big dispersion force is filled in after silane coupling agent is handled and shows high reinforcing in rubber, and heat aging performance is better than It is fast to extrude carbon black, but elasticity is worse than fast extrusion carbon black.The fast carbon black and precipitated silica mass ratio of extruding is 1:1, will be extruded fastly Carbon black and precipitated silica are used cooperatively as reinforcing agent, can take into account reinforcing effect and heat aging property.
No. 1 vulcanizing agent is matched with promotor, further increases the performance of carboxylic acid type acrylic rubber.Promotor is preferred For diphenylguanidine OTG.Wherein, No. 1 vulcanizing agent (hexamethylene diamine carbamate) is usually used in rubber and does vulcanizing agent, promotor DOTG refers to a kind of chemical substance that can be used for natural rubber, diene-based synthetic rubber, in the embodiment of the present invention, passes through No. 1 sulphur Agent is matched with promotor, and carboxylic acid type acrylic rubber obtained is made not only to have preferable compression set performance, Also there is preferable thermal stability, higher hardness and higher tensile strength simultaneously.
Further, silane coupling agent can improve dispersibility and bonding force of the filler in rubber, improve inorganic filler with Compatibility between rubber improves processing performance and improves the property such as machinery, electricity and the weatherability of filled plastics (including rubber) Energy.Silane coupling agent is selected from one of KH-550 and Si-69 in the embodiment of the present invention.
Further, processing aid is stearic acid, as vegetable oil system fatty acid, in the process of rubber, by one After certainty ratio addition, the dispersion for extruding carbon black and precipitated silica fastly can be conducive to, while softening and plasticising can also be played Effect can reduce the viscosity of sizing material, improves processing performance, is remarkably improved the plasticity of sizing material.
Further, what is be added in production process of the anti-aging agent in rubber can delay ageing of rubber, extension rubber to make With the chemicals in service life, wherein anti-aging agent is preferably TK-100.
A kind of preparation method of low compression set carboxylic acid type acrylic rubber, comprising the following steps:
By carboxylic acid type acrylic rubber, carbon black, precipitated silica, processing aid and anti-aging agent addition open mill are extruded fastly The first rubber compound is made in middle progress first time mixing.The embodiment of the present invention is kneaded specific step for the first time are as follows: (1) by cooperation Ratio has weighed carboxylic acid type acrylic rubber, has extruded carbon black, precipitated silica, processing aid and anti-aging agent fastly;(2) it opens Mill is pressed in stearic acid on roller, then in carboxylic acid type acrylic rubber investment roller, makes rubber bag roller, regulating roller Away from making to keep a small amount of gum deposit on roller;(3) fast carbon black, precipitated silica, the anti-aging agent of extruding is even added in roller and is carried out It is kneaded.When addition half extrudes carbon black and precipitated silica fastly, every side is carried out 3/4 cutter 1 time, and remaining fast extrusion is then added Carbon black and precipitated silica, every side carry out 3/4 cutter 2 times.
When the temperature of the first rubber compound is 50-70 DEG C, silane coupling agent is added, the second rubber compound is made;It is mixed first When the temperature of refining glue is 50-70 DEG C, the purpose that silane coupling agent is added is in order in shape carboxylic acid type acrylic rubber and hard charcoal Black while uniformly when being present in system, addition silane coupling agent links the both ends of silane coupling agent with two simultaneously Object (shape carboxylic acid type acrylic rubber and white carbon black) combines, when avoiding silane coupling agent pretreatment white carbon black, one end quilt In conjunction with other end by long-term vacant situation.Wherein, when silane coupling agent mixing is added, the temperature of the first rubber compound exists 50-70 DEG C, each strand has relatively high kinetic energy, this be conducive to silane coupling agent and rubber and white carbon black strand it is quick, Firm connection, greatly improves the coupling intensity between rubber and white carbon black, so that the reticular structure formed when the vulcanization of rubber Strand has better anti-pressure ability, improves the compression set performance of rubber.
Preferably, when the temperature of the first rubber compound is 65 DEG C, silane coupling agent is added.Second in the embodiment of the present invention The specific steps of mixing are as follows: when the temperature of the first rubber compound is 50-70 DEG C, silane coupling agent is added and is kneaded, every side carries out 3/4 Cutter 3 times, bottom sheet, clot thin logical 6 times, slice, cooling.
Then No. 1 vulcanizing agent and promotor is added, then carries out sulfidization molding, low compression set carboxylic acid type propylene is made Acid esters rubber.The specific steps of sulfidization molding are as follows: (1) vulcanizing agent and rush are added when the temperature of the second rubber compound is not higher than 50 DEG C Into agent, the thin logical, slice of clot is parked;(2) as bin aging 12h, white silk, clot thin logical 6 times, slice are then returned, on vulcanizer Vulcanization.
Embodiment 1
A kind of preparation method of low compression set carboxylic acid type acrylic rubber, comprising the following steps:
(1) following raw material is weighed by weight: ACM-120:100 parts of acrylic rubber;It is fast to extrude carbon black N-550:25 Part;Deposition white carbon black: 25 parts;Si-69:2 parts of silane coupling agent;TK-100:5 parts of anti-aging agent;Stearic acid: 2 parts;No. 1 vulcanizing agent: 1 part;OTG:2 parts of diphenylguanidine.
(2) open mill is opened, stearic acid is pressed on roller, then carboxylic acid type acrylic rubber is put into roller, Make rubber bag roller, regulating roller is away from making to keep a small amount of gum deposit on roller;
(3) fast carbon black, precipitated silica, the anti-aging agent of extruding is even added in roller and is kneaded, when addition half When fast extrusion carbon black and precipitated silica, every side is carried out 3/4 cutter 1 time, and remaining fast extrusion carbon black and precipitating hard charcoal is then added When black, every side is carried out 3/4 cutter 2 times, is all added in sizing material after the material for scattering inside receiver is swept up;
(4) when the temperature of the first rubber compound is 65 DEG C, it is slowly added into silane coupling agent;
(5) every side carries out 3/4 cutter 3 times, bottom sheet, clot thin logical 6 times, slice, cooling;
(6) be added No. 1 vulcanizing agent and diphenylguanidine OTG when the temperature of the second rubber compound is not higher than 50 DEG C, clot it is thin it is logical, Slice is parked;
(7) as bin aging 12h, white silk, clot thin logical 6 times, slice are then returned.
It will be tested after material cures obtained above, steps are as follows:
(1), vulcanize processing and fabricating vulcanization test piece and test block in sulfurizing mould.
(2), vulcanization test piece and test block are put into convection oven, are toasted 4 hours under the conditions of 170 DEG C, close baking oven electricity Source allows it to naturally cool to room temperature.
(3), test piece is parked by the regulation of rubber examination criteria.
(4), after parking the time as defined in arrival, performance Indexs measure is carried out to test piece.
(5), test block is put into compression set detection fixture, together with test piece, is put into ageing oven, Degradation is carried out under conditions of 150 DEG C × 70 hours.
Test result is as shown in table 1.
Embodiment 2
A kind of preparation method of low compression set carboxylic acid type acrylic rubber, comprising the following steps:
(1) following raw material is weighed by weight: ACM-220:100 parts of acrylic rubber;It is fast to extrude carbon black N-550:25 Part;25 parts of precipitated silica, Si-69:2 parts of silane coupling agent;TK-100:5 parts of anti-aging agent;Stearic acid: 2 parts;No. 1 vulcanizing agent 1 Part;2 parts of diphenylguanidine OTG;
With embodiment 1, testing result is as shown in table 1 for processing and detection method.
Embodiment 3
A kind of preparation method of low compression set carboxylic acid type acrylic rubber, comprising the following steps:
(1) following raw material is weighed by weight: ACM-320:100 parts of acrylic rubber;It is fast to extrude carbon black N-550:25 Part;Precipitated silica: 25 parts;, Si-69:2 parts of silane coupling agent;TK-100:5 parts of anti-aging agent;Stearic acid: 2 parts;No. 1 vulcanization Agent: 1 part, OTG:2 parts of diphenylguanidine;
With embodiment 1, testing result is as shown in table 1 for processing and detection method.
Comparative example 1 (variation carbon black combination, only extrude carbon black with fast)
A kind of preparation method of conventional carboxylic acid's type acrylic rubber, comprising the following steps:
(1) following raw material is weighed by weight: ACM-120:100 parts of acrylic rubber;It is fast to extrude carbon black N-550:50 Part;TK-100:5 parts of anti-aging agent;Stearic acid: 2 parts;No. 1 vulcanizing agent: 1.0 parts;DOTG:2.0 parts;
(2) open open mill, stearic acid is pressed on roller, then by carboxylic acid type acrylic rubber put into roller In, make rubber bag roller, regulating roller is away from making to keep a small amount of gum deposit on roller;
(3) fast extrusion carbon black, anti-aging agent are even added in roller and are kneaded, extrude carbon black fastly when half is added When, every side carries out 3/4 cutter 1 time, and when remaining fast extrusion carbon black is then added, every side is carried out 3/4 cutter 2 times;
(4) every side carries out 3/4 cutter 3 times, bottom sheet, clot thin logical 6 times, slice, cooling;
(5) be added No. 1 vulcanizing agent and diphenylguanidine OTG when the temperature of the second rubber compound is not higher than 50 DEG C, clot it is thin it is logical, Slice is parked;
(6) as bin aging 12h, white silk, clot thin logical 6 times, slice are then returned.
It will be tested after material cures obtained above, step is the same as embodiment 1.Testing result is as shown in table 1.
Comparative example 2 (changes carbon black combination, only use precipitated silica)
A kind of preparation method of conventional carboxylic acid's type acrylic rubber, comprising the following steps:
(1) following raw material is weighed by weight: ACM-120:100 parts of acrylic rubber;Precipitated silica: 50 parts; Si-69:2 parts of silane coupling agent;TK-100:5 parts of anti-aging agent;Stearic acid: 2 parts;No. 1 vulcanizing agent: 1.0 parts;DOTG:2.0 parts;
Silane coupling agent is directly added into white carbon black at normal temperature, is uniformly mixed, for use, processing and detection method are the same as real Example 1 is applied, testing result is as shown in table 1.
Comparative example 3 (room temperature addition silane coupling agent)
A kind of preparation method of common acrylic rubber containing active chlorine, comprising the following steps:
(1) following raw material is weighed by weight: ACM-120:100 parts of acrylic rubber;It is fast to extrude carbon black N-550:25 Part;Precipitated silica: 25 parts;Silane resin acceptor kh-550: 2 parts, TK-100:5 parts of anti-aging agent;Stearic acid: 2 parts;No. 1 vulcanization Agent: 1.0 parts;DOTG:2.0 parts.
(2) at room temperature, silane coupling agent is directly added into precipitated silica, is uniformly mixed, for use.
(3) open mill is opened, stearic acid is pressed on roller, then in rubber investment roller, makes rubber bag roller, regulating roller Away from making to keep a small amount of gum deposit on roller;
(4) fast carbon black, precipitated silica, the anti-aging agent of extruding is even added in roller and is kneaded, when addition half When fast extrusion carbon black and precipitated silica, every side is carried out 3/4 cutter 1 time, and remaining fast extrude in carbon black is then added and precipitates hard charcoal Black, every side carries out 3/4 cutter 2 times, is all added in sizing material after the material for scattering inside receiver is swept up;
(5) every side carries out 3/4 cutter 3 times, bottom sheet, clot thin logical 6 times, slice, cooling;
(6) vulcanizing agent is added when the temperature of rubber compound is not higher than 50 DEG C, the thin logical, slice of clot is parked;
(7) as bin aging 12h, white silk, clot thin logical 6 times, slice are then returned.
It will be tested after material cures obtained above, steps are as follows:
(1), vulcanize processing and fabricating vulcanization test piece and test block in sulfurizing mould.
(2), vulcanization test piece and test block are put into convection oven, are toasted 8 hours under the conditions of 170 DEG C, close baking oven electricity Source allows it to naturally cool to room temperature.
(3), test piece is parked by the regulation of rubber examination criteria.
(4), after parking the time as defined in arrival, performance Indexs measure is carried out to test piece.
(5), test block is put into compression set detection fixture, together with test piece, is put into ageing oven, Degradation is carried out under conditions of 150 DEG C × 70 hours.
Testing result is as shown in table 1.
Table 1
As it can be seen from table 1 the low compression set carboxylic acid type acrylic rubber of preparation of the embodiment of the present invention has Preferable hardness, elongation at break and higher tensile strength, while there is preferable compression set performance.
In conclusion the present invention provides a kind of low compression set carboxylic acid type acrylic rubber and preparation method thereof Beneficial effect is, wherein by extruding being used cooperatively for carbon black and deposition white carbon black fastly, while passing through No. 1 vulcanizing agent and promotion Agent is used cooperatively, and the carboxylic acid type acrylic rubber prepared is made to have preferable heat aging performance and compression set Energy;Silane coupling agent is added during rubber compounding, carboxylic acid type acrylic rubber and White Carbon black uniformly exist simultaneously In system, when addition, the both ends of silane coupling agent can avoid silane coupling agent and pre-process simultaneously with two objects ining conjunction with When White Carbon black, one end is combined, and other end is by long-term vacant situation, wherein when silane coupling agent mixing is added, first For the temperature of rubber compound at 50-70 DEG C, each strand has relatively high kinetic energy, this is conducive to silane coupling agent and rubber and White Carbon black Quick, the firm connection of strand, greatly improve the bond strength of the reticular structure strand formed when vulcanization, so that rubber Xanthan molecule has better anti-pressure ability, improves the compression set performance of carboxylic acid type acrylic rubber, makes finally to make The low compression set carboxylic acid type acrylic rubber obtained has preferable comprehensive performance.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (8)

1. a kind of low compression set carboxylic acid type acrylic rubber, it is characterised in that: its raw material includes: according to parts by weight 100 parts of carboxylic acid type acrylic rubber, fast extrusion carbon black 10-50 parts, 10-50 parts of precipitated silica, 1-5 parts of silane coupling agent, 1 Number 1-3 parts of vulcanizing agent, 2-6 parts of promotor, 1-3 parts of processing aid and 2-5 parts of anti-aging agent, the fast extrusion carbon black and described heavy The mass ratio of shallow lake white carbon black is 1:1, and the mass ratio of No. 1 vulcanizing agent and the promotor is 1:2.
2. low compression set carboxylic acid type acrylic rubber according to claim 1, it is characterised in that: the silane Coupling agent is selected from one of KH-550 and Si-69.
3. low compression set carboxylic acid type acrylic rubber according to claim 1, it is characterised in that: the promotion Agent is diphenylguanidine OTG.
4. low compression set carboxylic acid type acrylic rubber according to claim 1, it is characterised in that: the processing Auxiliary agent is stearic acid.
5. low compression set carboxylic acid type acrylic rubber according to claim 1, it is characterised in that: described anti-old Agent is TK-100.
6. a kind of preparation method of low compression set carboxylic acid type acrylic rubber as described in claim 1, feature It is: the following steps are included:
By the carboxylic acid type acrylic rubber, the fast extrusion carbon black, the precipitated silica, the processing aid and described Anti-aging agent, which is added in open mill, carries out first time mixing, and the first rubber compound is made;
When the temperature of the first rubber compound is 50-70 DEG C, the silane coupling agent is added, the second rubber compound is made;
Then No. 1 vulcanizing agent and promotor is added, then carries out sulfidization molding, the low compression set carboxylic acid type is made Acrylic rubber.
7. preparation method according to claim 6, it is characterised in that: when the temperature of the first rubber compound is 65 DEG C, be added The silane coupling agent.
8. preparation method according to claim 6, it is characterised in that: add when the temperature of the second rubber compound is not higher than 50 DEG C Enter the vulcanizing agent, then carries out sulfidization molding.
CN201910611537.4A 2019-07-08 2019-07-08 Low-compression permanent deformation carboxylic acid type acrylate rubber and preparation method thereof Active CN110330750B (en)

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CN113999473A (en) * 2021-11-30 2022-02-01 重庆长安汽车股份有限公司 High-temperature-resistant acrylate rubber and preparation method thereof
CN114790320A (en) * 2022-05-11 2022-07-26 山东海益橡胶科技有限公司 Low-viscosity high-strength acrylate rubber compound and preparation method thereof
CN114960241A (en) * 2022-04-29 2022-08-30 江苏赛福天钢索股份有限公司 High-temperature-resistant anti-aging steel wire rope and preparation method thereof

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