CN101555330B - Fiber reinforced rubber - Google Patents
Fiber reinforced rubber Download PDFInfo
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- CN101555330B CN101555330B CN2009100310115A CN200910031011A CN101555330B CN 101555330 B CN101555330 B CN 101555330B CN 2009100310115 A CN2009100310115 A CN 2009100310115A CN 200910031011 A CN200910031011 A CN 200910031011A CN 101555330 B CN101555330 B CN 101555330B
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Abstract
The invention relates to a fiber reinforced rubber, for which the strength can be remarkably improved, the permanent compression set can be reduced and the anti-tear performance of rubber sheet can be enhanced. A method for preparing the fiber reinforced rubber comprises the following steps: a. mastication of rubber; b. reinforcing filler, fiber and accessory ingredient are added into the rubber for mixing; wherein, the fiber and the reinforcing filler is evenly mixed to prepare pre-dispersoid, and the pre-dispersoid is added into the rubber. As a preferred proposal, the method adopts styrene-butadiene rubber, nitrile rubber and neoprene which have the good properties of wearing resistance, pressure resistance, oil and water resistance and air tightness resistance as the rubber. The rubber sheet produced by the method can work under ultra-high temperature and pressure in various media for a long time with the maximum working temperature being 300 DEG C, and maintains good elasticity, less compressive deformation and excellent physical and mechanical properties which are reduced by not more than 20% compared with those at the normal temperature.
Description
Technical field
The present invention relates to a kind of fiber reinforced rubber.
Background technology
Some conventional general purpose synthetic rubbers, as the rubber plate that butylbenzene, butyronitrile and chloroprene rubber are produced, its critical use temperature is respectively: 120 ℃, 140 ℃ and 160 ℃, because self characteristics, the working conditions in different media is subjected to strict restriction.When in media such as some High Temperature High Pressure, oil, solvent, soda acid, using, can occur prematurely that swelling, be full of cracks and compression set are big, physical and mechanical properties is obviously descended the degradation defective, when serious even can occur dissolving, lose some advantages that this highly elastic material of rubber is possessed fully.Especially ought be prepared into rubber plate, under hot environment, use, when being mainly used in container sealing, flange seal, require the better performances of its heat resisting and pressure resisting, anti-all kinds of SOLVENTS and chemical mediator, and requiring hardness height, the compression set of product little, its physical and mechanical properties and inherent elastic performance thereof can be kept when using in above environment.Known way is, according to different environments for use and medium requirement, by adjusting rubber compounding and adding some aramid fibers, synthon, carbon fiber, glass fibre etc., can improve the use range of general purpose synthetic rubber, increase the service life, still, effect is not very good, major cause is that fiber can't be uniformly dispersed in rubber, and and rubber between form bounding force preferably, make reinforced effects limited.A kind of known way is that fiber is dipped in the adhesive specially (i.e. " soaking paste ") in advance, re-use after the oven dry, because tackiness agent has certain surface modification effect to fiber, can improve fiber in rubber dispersed homogeneous degree and the bounding force between itself and the rubber, but effect still is not very good, gained rubber intensity and non-deformability can not satisfy service requirements, and work-ing life is shorter.
Summary of the invention
The invention provides a kind of fiber reinforced rubber, can significantly improve its intensity, reduce its compression set and increase the tear resistance of rubber plate, and when in oil, solvent (agent), fuel, water, low-pressure steam, coal gas, acid or alkali and non-attacking solution medium, using, can life-time service and stable performance excellence.
The preparation method of described fiber reinforced rubber comprises the steps:
A. rubber plastic steelmaking;
B. in rubber, add reinforcing filler, fiber, auxiliary agent, carry out mixing;
Wherein, fiber and reinforcing filler add in the rubber after making predispersion through mixing earlier again.
The present invention is on the prior art basis, reinforcing filler and fiber are mixed before mixing, make powdery reinforcing filler and fiber be in the relative separation state, make predispersion, carry out glue stuff compounding by its order of addition(of ingredients) then, fiber is disperseed in rubber equably, and improve the binding property between itself and the rubber, thereby make rubber significantly improve intensity, reduce compression set, increase the tear resistance of rubber.Omitted the pre-treatment step of using fibre-reinforced soaking paste, oven dry in the prior art, not only easy and simple to handle, reduced production cost; simultaneously; tackiness agent is a kind of known to the disagreeableness chemical feedstocks of environment, and therefore, the present invention is also very favourable to environment protection.
Wherein, the selecting for use of various raw materials, proportioning all can adopt the state of the art, and be definite through testing according to product requirement by those of ordinary skill in the art.
As preferred version, described rubber is styrene-butadiene rubber(SBR), paracril, chloroprene rubber.This different materials of styrene-butadiene rubber(SBR), paracril and chloroprene rubber, wear resistance, resistance to pressure, oil-proofness and water-fast, anti-resistance to air loss are good.
As preferred version, described fiber is the mixture of one or more arbitrary proportions in glass fibre, polypropylene fibre, aramid fiber, the carbon fiber.Wherein it is cheap and easy to get for glass fibre, and the heat resisting and pressure resisting excellent performance is selected for use usually based on the glass fibre enhancing, and the fiber that is equipped with unlike material reaches result of use.The direct over-all properties that influences rubber of ratio regular meeting that the fiber of different varieties is mixed.Described Fibre diameter 20-50 μ m, length 4-6mm.Above-mentioned fiber all has splendid electrical insulation capability, higher mechanical strength, excellent thermotolerance and anti-various chemical mediator corrodibility, and its intensity and Young's modulus are quite high, even exceed tens times and even hundred times of steel, and quality is 1/10th of a steel.So select for use above fiber in rubber, to strengthen, can greatly widen the use range of rubber plate, improve physical and mechanical properties, reduce compression set and increase tearing toughness.
Vulcanizing agent can be selected sulphur, ethylidine thiocarbamide (NA-22) for use.
Promoting agent can be selected zinc oxide, magnesium oxide, stearic acid for use.
Anti-aging agent can select 2,2 for use, 4-trimethylammonium-1,2 dihyaroquinoline polymer (hereinafter to be referred as RD), N-sec.-propyl-N-diphenyl-para-phenylene diamine (hereinafter to be referred as 4010NA).
Promotor can be selected dibenzothiazyl disulfide (DM), 2 one thiol groups and thiazole (M), tetramethyl-thiuram disulfide (TMTD) etc. for use.
Reinforcing filler can be selected white carbon black (SiO for use
2NH
2O), high abrasion furnace black, treated carbonates etc.
Preferred proportioning raw materials is: 80.0～90.0 parts in styrene-butadiene rubber(SBR), 20.0～10.0 parts of high styrene resins, 0.5～3.0 part of vulcanizing agent, 4.0～12.0 parts of promoting agents, 0.5～3.0 part of promotor, 1.0～2.0 parts in anti-aging agent, 40.0～80.0 parts of reinforcing fillers, 10.0～15.0 parts in glass fibre, 5.0～10.0 parts of polypropylene fibres.
Another kind of preferred proportioning raw materials is: 70.0～80.0 parts of paracrils, 30.0～20.0 parts of chlorinatedpolyethylenees, 0.5～3.0 part of vulcanizing agent, 5.0～11.0 parts of promoting agents, 1.5～3.0 parts of promotor, 1.0～2.0 parts in anti-aging agent, 40.0～80.0 parts of reinforcing fillers, 10.0～20.0 parts in glass fibre, 5.0～10.0 parts of aramid fibers.
Another kind of preferred proportioning raw materials is: 100.0 parts of chloroprene rubbers, 0.5～1.0 part of vulcanizing agent, 8.0～12.0 parts of promoting agents, 40.0～80.0 parts of reinforcing fillers, 10.0～20.0 parts in glass fibre, 15.0～30.0 parts on carbon fiber.
By the rubber plate that the present invention produced, hardness is 95 ± 5 degree, tensile strength at yield is 8～12MPa, tensile yield is 150～250%, compression set can be in superhigh-temperature and-pressure and the medium-term and long-term work of various medium less than 15%, and maximum operating temperature can reach 300 ℃, and keep good elasticity, lower compression set and excellent physical and mechanical performance, be no more than 20% with performance comparison decline normal temperature under.
Embodiment
Below in conjunction with embodiment this is elaborated clearly, can not limits right of the present invention place with this, the equivalent variations according to institute of the present invention claim is done still belongs to content that the present invention is contained.
Embodiment 1-9:
Proportioning raw materials by weight is as shown in table 1.Preparation process is as follows:
(1) with polypropylene fibre, glass fibre and white carbon black and treated carbonates together, in container, carries out high-speed stirring, make the predispersion of finely dispersed staple fibre and powder.
(2) styrene-butadiene rubber(SBR) and high styrene resin are put into moulded in the internal rubber mixer and refine, the time of plasticating is 5～6min, plasticating temperature is controlled at 120～130 ℃, adding promoting agent, promotor, anti-aging agent, tinting material and predispersion more successively carries out mixing, mixing time is not less than 15min, and melting temperature is controlled at below 130 ℃.
(3) be dumped into after the mixing end and add vulcanizing agent on the opening rubber mixing machine, the roller temperature should be controlled at below 100 ℃ when adding vulcanizing agent, to avoid incipient scorch.Unloading piece is cooled off, is parked then; Carry out the fast inspection of physical and mechanical properties during this period, check whether every index is qualified.
(4) rolling out film.The film of parking is after the assay was approved slightly refined and heat refining, on rolling press according to the required thickness of product, width and the even slice of length, moulding, and pass through vulcanizing press, vulcanized 15～20 minutes under 145 ℃～151 ℃ temperature, the operating pressure of 10～15MPa, the sheet material after sulfuration size in accordance with regulations carries out deburring, check, packing, warehouse-in and gets final product.
The raw materials used proportioning of table 1 embodiment 1-9
Embodiment 10-18:
Proportioning raw materials by weight is as shown in table 2.
The raw materials used proportioning of table 2 embodiment 10-18
Preparation process is as follows:
(1) with aramid fiber, glass fibre and white carbon black and treated carbonates together, in container, carries out high-speed stirring, make the predispersion of dispersed staple fibre uniformly and reinforcing filler.
(2) paracril carries out one, two sections low temperature thin-passes of low temperature and plasticates on opening rubber mixing machine, and the roller temperature control is at 50 ± 5 ℃, first section roll spacing 1～2mm that plasticates, and crossing the roller number of times is 25 times; Park and carry out second section after 8 hours and plasticate, roll spacing 1～2mm, crossing the roller number of times is 20 times, weighing is also parked stand-byly, the storage period should not be lower than 8 hours, is not higher than 72 hours, otherwise look plasticate invalid.The paracril that to plasticate and chlorinated polyethylene resin are put into and are moulded in the internal rubber mixer and refine then, the time of plasticating is 5～6min, plasticating temperature is controlled at 120～130 ℃, adding promoting agent, anti-aging agent, tinting material, predispersion and promotor more successively carries out mixing, mixing time is not less than 15min, and melting temperature is controlled at below 130 ℃.
(3) be dumped into after the mixing end and add vulcanizing agent on the opening rubber mixing machine, the roller temperature should be controlled at below 100 ℃ when adding vulcanizing agent, to avoid incipient scorch.Unloading piece is cooled off, is parked then; Carry out the fast inspection of physical and mechanical properties during this period, check whether every index is qualified.
(4) rolling out film.The film of parking is after the assay was approved slightly refined and heat refining, on rolling press according to the required thickness of product, width and the even slice of length, moulding, and pass through vulcanizing press, vulcanized 15～20 minutes under 145 ℃～151 ℃ temperature, the operating pressure of 10～15MPa, the sheet material after sulfuration size in accordance with regulations carries out deburring, check, packing, warehouse-in and gets final product.
Case study on implementation 19-21:
Proportioning raw materials by weight is as shown in table 3.Preparation process is as follows:
(1) with glass fibre and carbon fiber and high abrasion furnace black together, carries out high-speed stirring, make dispersed predispersion uniformly at container.
(2) chloroprene rubber thin-pass on opening rubber mixing machine is plasticated 20 times, the roller temperature control is at 50 ± 5 ℃, chloroprene rubber after plasticating is put in the Banbury mixer, the predispersion that adds promoting agent, fiber and strengthening agent successively carries out mixing, mixing time is not less than 15min, melting temperature is controlled at below 130 ℃.
(3) mixing being dumped into after evenly adds vulcanizing agent in the mill, and the roller temperature should be controlled at below 100 ℃ when adding vulcanizing agent, to avoid incipient scorch.The unloading piece cooling is parked then, carries out the fast inspection of physical and mechanical properties during this period, checks whether every index is qualified.
(4) rolling out film.The film of parking is after the assay was approved slightly refined and heat refining, on rolling press according to the required thickness of product, width and the even slice of length, moulding, and pass through vulcanizing press, vulcanized 15～20 minutes under 145 ℃～151 ℃ temperature, the operating pressure of 10～15MPa, the sheet material after sulfuration size in accordance with regulations carries out deburring, check, packing, warehouse-in and gets final product.
The raw materials used proportioning of table 3 embodiment 19-21
Comparative examples
Proportioning raw materials is as shown in table 4, and preparation process is as follows: earlier natural rubber is broken glue on opening rubber mixing machine, roll spacing is controlled at 3～4mm when breaking glue, and the roller temperature is 40～50 ℃.The adjustment roll spacing is 1～2mm, thin-pass is carried out in broken good natural rubber input plasticate on opening rubber mixing machine, and the roller temperature control is at 50 ℃ ± 5 ℃, and crossing the roller number of times is 25 times; Then the cooling park, the storage period can not be less than 8 hours, no more than 72 hours, otherwise be considered as invalid.Natural rubber after parking plasticating and tread reclaimed rubber are put into and are carried out in the internal rubber mixer and refine, and the refining time is 3-4 minute, add promoting agent, promotor, reinforcing filler etc. then successively and carry out mixingly, melting temperature is controlled at 125～135 ℃, and the time is not less than 10min.Mixing end back discharging adds vulcanizing agent on opening rubber mixing machine, the roller temperature should be controlled at below 100 ℃ when adding vulcanizing agent, to avoid incipient scorch.Unloading piece is cooled off, is parked then; Carry out the fast inspection of physical and mechanical properties during this period, check whether every index is qualified.To park during rolling out film and work in-process sizing material after the assay was approved, and slightly refine earlier and heat refining, thickness, length and the width by product is carried out to a slice again.Enter flat vulcanizer at last, 135～through 142 ℃ temperature, 600～800T (after please being converted into the time of sulfuration under the operating pressure of Pa or 10～15MPa) and 3～5 minutes, carry out deburring, check, packing warehouse-in, promptly can be made into General Purpose Rubber sheet material.
Table 4
Embodiment 1-21 gained rubber plate and comparative examples gained General Purpose Rubber plate property to such as the table 5-7 shown in.
Table 5
| Maximum operation (service) temperature (℃) | Hardness (that A degree continues) | Tensile strength at yield (MPa) | Tensile yield (%) | Compression set (%) | |
| Contrast | 80 | 75 | 2.1 | 150 | 40 |
| Embodiment 1 | 200 | 92 | 9.0 | 210 | 13 |
| Embodiment 2 | 230 | 95 | 10.5 | 180 | 12 |
| Embodiment 3 | 230 | 97 | 10.8 | 150 | 11 |
| Embodiment 4 | 180 | 90 | 8.3 | 220 | 14 |
| Embodiment 5 | 180 | 93 | 9.5 | 200 | 13 |
| Embodiment 6 | 190 | 95 | 10.0 | 180 | 12 |
| Embodiment 7 | 180 | 90 | 8.0 | 230 | 15 |
| Embodiment 8 | 180 | 92 | 8.8 | 220 | 15 |
| Embodiment 9 | 190 | 93 | 9.6 | 200 | 14 |
| Embodiment 10 | 210 | 93 | 9.5 | 230 | 13 |
| Embodiment 11 | 230 | 95 | 10.8 | 200 | 12 |
| Embodiment 12 | 220 | 97 | 11.2 | 180 | 11 |
| Embodiment 13 | 190 | 92 | 8.7 | 240 | 12 |
| Embodiment 14 | 200 | 93 | 9.8 | 220 | 10 |
| Embodiment 15 | 220 | 95 | 10.4 | 200 | 9 |
| Embodiment 16 | 200 | 90 | 8.3 | 250 | 15 |
| Embodiment 17 | 210 | 91 | 8.9 | 230 | 13 |
| Embodiment 18 | 220 | 94 | 9.6 | 210 | 12 |
| Embodiment 19 | 200 | 92 | 8.5 | 250 | 15 |
| Embodiment 20 | 260 | 95 | 10.3 | 230 | 13 |
| Embodiment 21 | 250 | 98 | 11.0 | 200 | 11 |
Table 6
Table 7
Claims (6)
1. fiber reinforced rubber, it is characterized in that being made by weight by following raw material: 80.0～90.0 parts in styrene-butadiene rubber(SBR), 20.0～10.0 parts of high styrene resins, 0.5～3.0 part of vulcanizing agent, 4.0～12.0 parts of promoting agents, 0.5～3.0 part of promotor, 1.0～2.0 parts in anti-aging agent, 40.0～80.0 parts of reinforcing fillers, 10.0～15.0 parts in glass fibre, 5.0～10.0 parts of polypropylene fibres, its preparation method comprises the steps:
A. rubber plastic steelmaking;
B. in rubber, add reinforcing filler, fiber, auxiliary agent, carry out mixing;
Fiber and reinforcing filler add in the rubber after making predispersion through mixing earlier again.
2. fiber reinforced rubber as claimed in claim 1 is characterized in that described Fibre diameter 20-50 μ m, length 4-6mm.
3. fiber reinforced rubber, it is characterized in that being made by weight by following raw material: 70.0～80.0 parts of paracrils, 30.0～20.0 parts of chlorinatedpolyethylenees, 0.5～3.0 part of vulcanizing agent, 5.0～11.0 parts of promoting agents, 0.5～2.5 part of promotor, 1.0～2.0 parts in anti-aging agent, 40.0～80.0 parts of reinforcing fillers, 10.0～20.0 parts in glass fibre, 5.0～10.0 parts of aramid fibers, its preparation method comprises the steps:
A. rubber plastic steelmaking;
B. in rubber, add reinforcing filler, fiber, auxiliary agent, carry out mixing;
Fiber and reinforcing filler add in the rubber after making predispersion through mixing earlier again.
4. fiber reinforced rubber as claimed in claim 3 is characterized in that described Fibre diameter 20-50 μ m, length 4-6mm.
5. fiber reinforced rubber, it is characterized in that being made by weight by following raw material: 100.0 parts of chloroprene rubbers, 0.5～1.0 part of vulcanizing agent, 8.0～12.0 parts of promoting agents, 40.0～80.0 parts of reinforcing fillers, 10.0～20.0 parts in glass fibre, 15.0～30.0 parts on carbon fiber, its preparation method comprises the steps:
A. rubber plastic steelmaking;
B. in rubber, add reinforcing filler, fiber, auxiliary agent, carry out mixing;
Fiber and reinforcing filler add in the rubber after making predispersion through mixing earlier again.
6. fiber reinforced rubber as claimed in claim 5 is characterized in that described Fibre diameter 20-50 μ m, length 4-6mm.
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| CN2009100310115A CN101555330B (en) | 2009-04-22 | 2009-04-22 | Fiber reinforced rubber |
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| CN2009100310115A CN101555330B (en) | 2009-04-22 | 2009-04-22 | Fiber reinforced rubber |
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| CN101555330B true CN101555330B (en) | 2011-08-31 |
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