CN105504544A - Acid-resisting low-compression permanent set rubber composite material and preparing method - Google Patents
Acid-resisting low-compression permanent set rubber composite material and preparing method Download PDFInfo
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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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
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- C—CHEMISTRY; METALLURGY
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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
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K5/00—Use of organic ingredients
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- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34924—Triazines containing cyanurate groups; Tautomers thereof
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention provides an acid-resisting low-compression permanent set rubber composite material. The composite material is prepared from, by mass, 100 parts of ethylene-propylene-diene monomer rubber, 2-4 parts of vulcanizing agent bi(tert-butyl peroxy) diisopropyl benzene of an peroxide vulcanization system, 0.5-2 parts of an assistant vulcanizing agent triallyl isocyanurate, 28 parts of activator zinc oxide, 0.5-2 parts of a processing agent stearic acid, 0-20 parts of inertia inorganic filler carbon black N990, 0-25 parts of silica powder and 0-10 parts of barium sulfate. The invention further provides a preparing method of the acid-resisting low-compression permanent set rubber composite material. Compared with fluororubber, the ethylene-propylene-diene monomer rubber is easier to process, monomers are low in price, easy to obtain and low in cost, the ethylene-propylene-diene monomer rubber has excellent water and steam resistance which is not possessed by fluororubber, it is unnecessary to add an acid acceptor in the formula, and therefore the composite material is more suitable for being used in an acid steam or liquid environment.
Description
Technical field
The present invention relates to a kind of acidproof and the formula of low compression set deformation rubber composite and preparation method, the formulating of recipe of the cross-linked rubber system particularly based on terpolymer EP rubber and preparation method.
Background technology
Rubber because there is snappiness, low modulus, the feature such as wear-resisting, density I is filled in a large number and be widely used in every field.Sizing material is shaped to various pressing through hot-press vulcanization, as seal washer, and bumper and absorbing shock pad etc.; Sebific duct and the section bar of different bore can be extruded by forcing machine.
For sealing article field, because it has good processibility, lower Compression Set, widely environmental compatibility, rubber product occupies important one seat.As common water tumbler, the sealing-ring of lunch box, the sealed strip of mechanical means, oil sealing etc.According to different practical service environments, relatively more conventional caulking gum has silicon rubber, paracril, terpolymer EP rubber, viton, the hot rubber in sky, urethanes etc.
But have a strong impact on rubber use range using the ageing of rubber occurred in even storage.Usually can with some significant phenomenons in weathering process, deliquescing, stickness, variable color, deformation cannot be replied, and becomes fragile, hardening, be full of cracks etc.In physicals, rubber has the change of swelling, rheological property etc.Mechanical property can occur the indexs such as tensile strength, elongation at break, shock strength, flexural strength, rate of compression, elasticity decline.This mainly owing to being heated for a long time, oxygen, light, mechanical force, radiation, chemical mediator, the external factor such as ozone in air effect, make elastomeric material macromolecular chain generation chemical transformation, destroy the original chemical structure of rubber, thus cause rubber performance to degenerate, simultaneously wherein the precipitation of unstable auxiliary agent also can cause the change of overall performance and the pollution of environment for use to external world.
Along with the destruction of chemical structure, rubber Compression Set increases, and sealing was lost efficacy gradually, brings greatly inconvenience and impact to production and life.Especially at sour environment etc. compared with the caulking gum used under severe environment, its life-span often can not meet the demands, as in the sour environment of Proton Exchange Membrane Fuel Cells inside the silicon rubber sealing material that uses, degrade after battery over multiple cycles discharge and recharge, Compression Set increases, rebound resilience reduces, and seal failure, causes the faults such as battery short circuit.Then price is higher compared with other rubber for the viton of chemical property excellence, and the vulcanization system of uniqueness is also unfavorable for and other rubber covulcanization, the acid-acceptor system adopted easily is drawn out of under sour environment, environment for use is polluted, its Compression Set is comparatively large simultaneously, and sealing effectiveness is not ideal enough.
Summary of the invention
In order to overcome the deficiency of existing rubber packing material acid resistance and compression permanentset performance, the present invention adopts a kind of composite system based on rubber newly, coordinate novel contour machining procedure, obtain a kind of acidproof and rubber packing material of low compression set.
The object of the invention is to be achieved through the following technical solutions:
A kind of acidproof low compression set rubber composite, it is composed of the following components:
By quality ratio:
Terpolymer EP rubber 100 parts;
Vulcanizing agent dual-tert-butyl dicumyl peroxide 2-4 part of peroxide vulcanizing system, cocuring agent cyanacrylate (0.5-2 part);
Activator 28 parts;
Processing aid stearic acid 0.5-2 part;
Inert inorganic filler carbon black N9900-20 part, silicon beautiful powder sillitin0-25 part, barium sulfate 0-10 part.
Main rubber material of the present invention is terpolymer EP rubber, and with ethylidene norbornene (ENB) for Third monomer, content is 4% ~ 6%, and molecular weight distribution is controlled long-chain branch (CLCB), and ethylene content is 50% ~ 70%.The concrete trade mark of described terpolymer EP rubber includes but not limited to Keltan6550, Keltan2650.
In filler, the beautiful powder of silicon is a kind of mushy natural microparticle, the inorganic mineral be made up of quasi spherical granular quartz and Schistose kaolinite, and two kinds of natural combinations of difform mineral define a kind of loose grain sheet lamination pattern structure, there is super-high fluidity and the dispersing property of other fillers more than 2 times, good insulating, hardness is large, unreactiveness, acid-fast alkali-proof, uvioresistant, pH value is in neutral, and specific refractory power is substantially identical with paint base.Be added in rubber matrix and have excellent dispersing property, soilless sticking is inclined to, good insulation preformance, and ageing resistance is good, the features such as anti-settling performance is good, and acid-fast alkali-proof weather resistance is good, and extrusion performance is good.Shaping rear dimensional stability is high, and little on hardness impact, compression set is very low, and perception fullness ratio is good, and sense of touch is soft and smooth, and overall appearance class is high.
The present invention also provides a kind of preparation method of acidproof low compression set rubber composite, and it comprises the following steps:
Sizing material room temperature in two roller mill of getting above-mentioned formula is carried out mixing, then rubber unvulcanizate is carried out pressing plate sulfuration on vulcanizing press; Post vulcanization is carried out after cross-linked rubber room temperature being parked 24h after traditional molded vulcanization; After reaching the post vulcanization time, close heating, continue air blast, allow rubber Temperature fall to room temperature.
The object of post vulcanization improves cross-linked network structure further, eliminate small molecule by-product, reduce Compression Set, improve shaping after stability.Post vulcanization completes in electric heating convection oven, with the carrying of tetrafluoroethylene pad, while ensureing to be heated evenly, avoids contacting with metal sheet, sticks together.After reaching the post vulcanization time, close heating, continue air blast, allow rubber Temperature fall to room temperature, reduce internal stress and produce and dimensional contraction.
In the process of described post vulcanization, utilize air blast to take away the small molecule by-product of generation fast simultaneously, avoid surperficial bloom phenomenon to occur.
Relative to prior art, advantage of the present invention comprises:
Because ethylene-propylene rubber(EPR) molecular chain has the saturability of height, make it have the performances such as excellent high temperature resistant, ageing-resistant, resistance to ozone, chemicals-resistant, resistance to vapor permeability and electrical isolation.Compared with viton, terpolymer EP rubber is more easily processed, and monomer is cheap and easy to get, cost is lower, it has the water-fast and water-fast steam performance of excellence not available for viton simultaneously, and does not need in formula to add acid-acceptor, uses under being more adapted at acid vapors or liquid environment.
Embodiment
Embodiment 1
Select terpolymer EP rubber (Keltan2650) 100 parts as matrix, add carbon black N990 (filler) 20 parts, dual-tert-butyl dicumyl peroxide (vulcanizing agent) 3 parts, cyanacrylate (cocuring agent) 1 part, 5 parts, zinc oxide (activator), stearic acid (processing aid) 0.5 part, in two roller mill, 80 DEG C of mixing 15 ~ 20 minutes slices, obtained rubber unvulcanizate; Vulcanizing press carries out pressing plate sulfuration, and cure conditions is 170 DEG C, 10 minutes, 16Mpa; Park after 24 hours and carry out post vulcanization, condition is 150 DEG C, 2 hours.
Embodiment 2
Select terpolymer EP rubber (Keltan6550) 100 parts as matrix, add 25 parts, the beautiful powder of silicon, dual-tert-butyl dicumyl peroxide (vulcanizing agent) 3 parts, cyanacrylate (cocuring agent) 1 part, 5 parts, zinc oxide (activator), stearic acid (processing aid) 0.5 part, in two roller mill, 80 DEG C of mixing 15 ~ 20 minutes slices, obtained rubber unvulcanizate; Vulcanizing press carries out pressing plate sulfuration, and cure conditions is 170 DEG C, 10 minutes, 16Mpa; Park after 24 hours and carry out post vulcanization, condition is 150 DEG C, 2 hours.
Embodiment 3
Select terpolymer EP rubber (Keltan6550) 100 parts as matrix, add 10 parts, barium sulfate, 10 parts, the beautiful powder of silicon, dual-tert-butyl dicumyl peroxide (vulcanizing agent) 3 parts, cyanacrylate (cocuring agent) 1 part, 5 parts, zinc oxide (activator), stearic acid (processing aid) 0.5 part, 2,2,4-trimethylammonium-1,2-dihyaroquinoline polymer (anti-aging agent) 2 parts, 2-mercaptobenzimidazole (anti-aging agent) 1 part, in two roller mill, 80 DEG C of mixing 15 ~ 20 minutes slices, obtained rubber unvulcanizate; Vulcanizing press carries out pressing plate sulfuration, and cure conditions is 170 DEG C, 10 minutes, 16Mpa; Park after 24 hours and carry out post vulcanization, condition is 150 DEG C, 2 hours.
The performance comparison of table 1: embodiment 1-3 and comparative example 1,2 is as follows:
Comparative example 1 is the terpolymer EP rubber of non-post vulcanization, formula and other conditions identical with embodiment 1.
Comparative example 2 is commercial viton FE2604, fills a prescription as FE2604100 part, vulcanizing agent bisphenol AF 3 parts, cocuring agent BPP 2 parts, 10 parts, acid-acceptor calcium hydroxide, carbon black 20 parts.Curing temperature 170 DEG C, post vulcanization condition: 250 DEG C, 10 hours.
Sour environment to be pH be 3 acidic solution, containing 2ppmHF and 10ppmH
2sO
4, formulated with deionized water; Probe temperature is 80 DEG C, to accelerate aging speed.
Vulcanization curve test adopts R100E type vulcanization of rubber instrument to test, and condition is 170 DEG C of X30min.Outcome record comprises: minimum torque (ML), the highest moment of torsion (MH), time of scorch (T10), sulfurizing time (T90).Probe temperature is 170 DEG C, and the test duration is 30 minutes.Test sample is 15 ~ 20g rubber unvulcanizate.
Hardness adopts LX-A type durometer, and specification is 0 ~ 100HA, and test result is ShoreA hardness, tests and carries out in strict accordance with ASTMD2240 standard.
Test the Compression Set of sample according to ASTM-D395, select MethodB, rate of compression is 25%, and test condition selects 125 DEG C of X22h.Test sample is the cross-linked rubber parked after post vulcanization more than more than 24h, and sample size is the right cylinder of diameter 29mm, high 12.5mm, is shaping with corresponding mould direct pressing, without cutting out.Often organize test 3 samples, test result gets its mean value.
High precision Density Measuring Instrument (D=0.0001g/cm
3), be mainly used in testing aging front and back elastomeric material sample quality and volume change, simultaneously for testing blended sample rate, concrete formula is as follows:
In formula:
△ M-quality change, %;
M
1the initial mass that-sample is tested in atmosphere, g;
M
2-sample aging after the quality of testing in atmosphere, g.
In formula:
△ V-volume change, %;
M
1the initial mass that-sample is tested in atmosphere, g;
M
2the initial mass that-sample is tested in water, g;
M
3-sample aging after the quality of testing in atmosphere, g;
M
4-sample aging after the quality of testing in water, g.
From test result, without the terpolymer EP rubber of post vulcanization, acid resistance is poor, and Compression Set is large.
Compared with commodity viton, the performance of the terpolymer EP rubber after post vulcanization is suitable with it, and Compression Set is less, and hardness is also less.Add the terpolymer EP rubber of the beautiful powder of silicon, Compression Set obviously reduces, and acid resistance also increases.Add anti-aging agent and barium sulfate filler further, the acid resistance of terpolymer EP rubber system has clear improvement, considerably beyond price viton costly.
Described ternary ethlene propyene rubbercompound material well solves the problem of the acid resistance deficiency of sealing material, has lower hardness and Compression Set simultaneously, can realize identical sealing effectiveness under lower encapsulation pressure.And price is cheap, raw material is easy to get, and complete processing is comparatively simple, is applicable to continuous seepage in enormous quantities.
It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (5)
1. an acidproof low compression set rubber composite, is characterized in that: it is made up of the component of following mass ratio:
Terpolymer EP rubber 100 parts;
Vulcanizing agent dual-tert-butyl dicumyl peroxide 2-4 part of peroxide vulcanizing system, cocuring agent cyanacrylate (0.5-2 part);
Activator 28 parts;
Processing aid stearic acid 0.5-2 part;
Inert inorganic filler carbon black N9900-20 part, silicon beautiful powder 0-25 part, barium sulfate 0-10 part.
2. acidproof low compression set rubber composite according to claim 1, is characterized in that:
In described terpolymer EP rubber, with ethylidene norbornene (ENB) for Third monomer, content is 4% ~ 6%, and molecular weight distribution is controlled long-chain branch (CLCB), and ethylene content is 50% ~ 70%.
3. acidproof low compression set rubber composite according to claim 1, is characterized in that: the model of described terpolymer EP rubber is Keltan6550 or Keltan2650.
4. a preparation method for acidproof low compression set rubber composite according to claim 1, is characterized in that: it comprises the following steps:
The all components getting formula ratio carries out mixing as sizing material room temperature in two roller mill, then rubber unvulcanizate is carried out pressing plate sulfuration on vulcanizing press; Post vulcanization is carried out after cross-linked rubber room temperature being parked 24h after traditional molded vulcanization; After reaching the post vulcanization time, close heating, continue air blast, make rubber Temperature fall to room temperature.
5. preparation method according to claim 4, is characterized in that: in the process of described post vulcanization, utilizes air blast to take away the small molecule by-product of generation fast simultaneously, avoids surperficial bloom phenomenon to occur.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116731405A (en) * | 2023-06-28 | 2023-09-12 | 中策橡胶集团股份有限公司 | Tire cord fabric sizing composition, mixing method thereof and all-steel radial tire |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116731405A (en) * | 2023-06-28 | 2023-09-12 | 中策橡胶集团股份有限公司 | Tire cord fabric sizing composition, mixing method thereof and all-steel radial tire |
| CN116731405B (en) * | 2023-06-28 | 2024-05-31 | 中策橡胶集团股份有限公司 | Tire cord fabric sizing composition, mixing method thereof and all-steel radial tire |
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