JP2001206987A - Rubber composition, layered product and hose - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an inexpensive hose excellent in oil resistance/heat resistance, retaining adhesion to a different kind of rubber excellent in heat resistance by using an inexpensive non-halogenated rubber material having improved performance in versatile fields such as oil resistance/heat resistance or the like. SOLUTION: This rubber composition comprising a blended material having a fixed blending ratio of a nitrile based rubber such as a NBR or the like and an EPDM compounded with an organic peroxide, sulfur or a vulcanization accelerator in a specific amount, and a layered product and a hose using the same.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a nitrile rubber (particularly, acrylonitrile-butadiene rubber or NB).
R) A rubber composition obtained by adding a predetermined component to a blended material of EPDM, a rubber composition layer and an acrylic rubber layer, a nitrile rubber layer, an epichlorohydrin rubber layer, and a chlorinated polyethylene using the rubber composition. The present invention relates to a laminate obtained by laminating and adhering a rubber layer or a chlorosulfonated polyethylene rubber layer, and a hose using the laminate. The use of the laminate and the hose is not limited, but is particularly suitable for an air hose or an oil hose of an automobile or the like.

[0002]

2. Description of the Related Art In recent years, the demand for higher performance of rubber materials for various uses has become more stringent year by year, and in particular, rubber parts for automobiles are required to be maintenance-free during a period of, for example, 10 years / 160,000 km. ing.

[0003] In order to satisfy the above requirements, halogen-containing rubber materials such as chloroprene rubber (CR) and epichlorohydrin rubber (ECO) generally exhibiting excellent performances in terms of heat resistance, oil resistance, ozone resistance and the like. The cases used are increasing, for example, in air hoses, oil hoses, other automotive hoses and industrial hoses,
Assuming that the hose structure is laminated, these halogen-containing rubber materials are often used as a cover material of a hose outer layer (in some cases, a hose inner surface material).

[0004]

However, the demand for the high performance of the rubber material does not permit the accompanying increase in cost, but rather demands the cost to be maintained or reduced. The above-mentioned halogen-containing rubber material (especially ECO) does not meet requirements in terms of cost. In addition, halogen-containing rubber materials (especially chlorine-containing rubber materials) are feared to affect the environment when incinerated and disposed.

In terms of performance itself, CR and E
CO is often problematic in that storage stability of unvulcanized rubber, compression set (C. Set) important for hose sealing performance, and low-temperature embrittlement are poor.

Accordingly, the present invention relates to a non-halogenated rubber material, which is characterized by the above heat resistance, oil resistance and ozone resistance.
Higher performance equal to or better than R and ECO can be realized while maintaining cost or lowering cost. In addition, it is possible to improve the adhesiveness with the mating material corresponding to the hose structure laminate. It is an object of the present invention to provide an excellent material, and to provide an advantageous laminate and a hose using the material.

The inventor of the present application has found that nitrile rubber and EPDM
When a specific vulcanizing system is used as a base material with a specific blend ratio and a specific vulcanizing system under a specific quantitative limitation, it is found that the above problem can be solved. Thus, the present invention has been completed.

[0008]

Means for Solving the Problems (Structure of the First Invention) The structure of the first invention of the present application (the invention of claim 1) for solving the above-mentioned problems is that a nitrile rubber and EPDM (ethylene-propylene-ethylene) are used. Diene terpolymer rubber) and nitrile rubber: EPDM = 70: 30 to 40:60, and 100 parts by weight of the blended material blended in a ratio of 70 to 40:60 with respect to 100 parts by weight of: Has been added,
It is a rubber composition. (1) Organic peroxide: 0.5 to 10 parts by weight. (2) Sulfur or vulcanization accelerator: 0.3 to 5 parts by weight.

(Structure of the Second Invention) The structure of the second invention of the present application (the invention according to claim 2) for solving the above problems is as follows.
The hydrotalcite compound is further added to the rubber composition according to the first invention in an amount of 1 to 100 parts by weight of the blend material.
20 parts by weight of a rubber composition.

(Structure of Third Invention) The structure of the third invention of the present application (the invention according to claim 3) for solving the above problems is as follows.
A laminate obtained by laminating and bonding a rubber composition layer using the rubber composition according to the first invention or the second invention, and a rubber material layer using an acrylic rubber with or without a reinforcing layer. is there.

(Structure of the Fourth Invention) The structure of the fourth invention of the present application (the invention according to claim 4) for solving the above problems is as follows.
The rubber composition layer using the rubber composition according to the first invention or the second invention and a rubber material layer using a nitrile rubber are laminated and bonded with or without a reinforcing layer. is there.

(Structure of Fifth Invention) The structure of the fifth invention of the present application (the invention according to claim 5) for solving the above problems is as follows.
A laminated body in which a rubber composition layer using the rubber composition according to the first invention or the second invention and a rubber material layer using epichlorohydrin rubber are laminated and adhered with or without a reinforcing layer. is there.

(Structure of the Sixth Invention) The structure of the sixth invention of the present application (the invention according to claim 6) for solving the above problems is as follows.
A laminate in which a rubber composition layer using the rubber composition according to the first invention or the second invention and a rubber material layer using a chlorinated polyethylene rubber are laminated and bonded with or without a reinforcing layer. Body.

(Structure of the Seventh Invention) The structure of the seventh invention (the invention according to claim 7) for solving the above problems is as follows.
A rubber composition layer using the rubber composition according to the first invention or the second invention, and a rubber material layer using a chlorosulfonated polyethylene rubber were laminated and bonded with or without a reinforcing layer, It is a laminate.

(Structure of Eighth Invention) The structure of the eighth invention (the invention according to claim 8) for solving the above problems is as follows.
Using the laminate according to any one of the third invention to the seventh invention,
It is a hose.

[0016]

[Operations and effects of the invention] (Operations and effects of the first invention) In general, nitrile rubbers represented by NBR are excellent in oil resistance to oils such as engine oil and gasoline, but have high heat resistance and ozone resistance. EPDM is inferior in oil resistance but has good heat resistance and ozone resistance. Therefore, the nitrile rubber and EPDM are firstly combined.
Nitrile rubber: EPDM = 70: 30-
By blending in a ratio within the range of 40:60,
It is possible to achieve a good balance between oil resistance, heat resistance, and ozone resistance.

Further, the blended material comprising nitrile rubber and EPDM, both of which are inexpensive non-halogenated materials, is extremely advantageous in terms of cost as compared with halogen-containing rubber materials such as ECO, and is incinerated and discarded. In some cases, there is no environmental impact based on halogens such as chlorine. Further, as described above, there are no problems in storage stability, compression set (C.Set), low-temperature embrittlement, and the like of unvulcanized rubber, which are likely to be found in halogen-containing rubber materials.

As is well known, EPDM does not cause a decrease in the flexibility of the hose even though it is heat-resistant. Therefore, the use of the above blend material is also effective for improving the heat resistance and dynamic ozone property of the hose. .

On the other hand, since EPDM has a property that it has poor reactivity with other kinds of rubbers, it is considered that a blended material layer containing the same has poor vulcanization adhesion with other material layers in a laminate as it is. . However, the above blend material 10
When a vulcanization system comprising (1) 0.5 to 10 parts by weight of an organic peroxide and (2) 0.3 to 5 parts by weight of sulfur or a vulcanization accelerator with respect to 0 parts by weight is used. It has been found that excellent vulcanization adhesive strength can be realized, and heat resistance and compression set can be improved by adding an organic peroxide, and initial elongation can be improved by adding sulfur or a vulcanization accelerator.

When the blending ratio of EPDM in the blending material is less than 30% by weight, the ozone property of the blending material is deteriorated, and when the blending ratio exceeds 60% by weight, the oil resistance is deteriorated. Next, if the added amount of the organic peroxide is less than 0.5 part by weight with respect to 100 parts by weight of the blend material, the vulcanization of the rubber may be insufficient, and
If the amount exceeds the weight part, the storage stability of the unvulcanized rubber is particularly deteriorated, and the vulcanization of the rubber is excessively advanced, so that the material of the blend material is hardened and the initial elongation may be reduced. If the amount of sulfur or the vulcanization accelerator is less than 0.3 parts by weight based on 100 parts by weight of the blended material, the initial elongation of the blended material may be reduced. If it exceeds, the scorch property will deteriorate and cause "burn",
Heat resistance may be slightly deteriorated.

(Function / Effect of the Second Invention) In the second invention, the hydrotalcite compound is further added to the rubber composition in an amount of 1 to 20 parts by weight based on 100 parts by weight of the blend material. The effect of further improving the heat resistance is obtained. If the addition amount of the hydrotalcite compound is less than 1 part by weight, the effect of the addition may not be sufficiently exhibited. If the addition amount exceeds 20 parts by weight, the material of the blend material becomes hard and the initial elongation increases. There is a risk of lowering.

(Functions and Effects of Third to Seventh Inventions) First
The rubber composition layer using the rubber composition according to the invention or the second invention is an inexpensive and advantageous material such as acrylic rubber and nitrile rubber while maintaining the good performance of the rubber compositions listed above. It can be firmly laminated and adhered to a rubber material layer using epichlorohydrin rubber, chlorinated polyethylene rubber or chlorosulfonated polyethylene rubber with or without a reinforcing layer.

Therefore, according to the third to seventh aspects of the present invention, the rubber material layer is inexpensive, has excellent heat resistance, oil resistance, etc., and is unique to an acrylic, nitrile, epichlorohydrin, chlorinated polyethylene or chlorosulfonated polyethylene rubber layer. And a laminate having excellent adhesiveness can be provided.

(Effect of the Eighth Invention) In the eighth invention, a hose having the same features as the above-mentioned laminated body by forming a hose using the laminated body according to the third to seventh aspects of the present invention. Can be provided.

[0025]

Next, embodiments of the first to eighth inventions will be described. In the following, simply "the present invention"
When it says, it points out 1st invention-8th invention collectively.

[Rubber Composition] The rubber composition according to the present invention basically comprises 0.5 to 10 parts by weight of an organic peroxide with respect to 100 parts by weight of a blend material of a nitrile rubber and EPDM. It contains 0.3 to 5 parts by weight of sulfur or a vulcanization accelerator.

[Blend Material] The blend ratio of the nitrile rubber and EPDM constituting the blend material is in the range of nitrile rubber: EPDM = 70: 30 to 40:60. The types of the nitrile rubber and EPDM are not limited, but preferably, NBR is used as the nitrile rubber,
AN amount as EPDM (content of bound acrylonitrile)
Is 31 to 50% by weight.

As a blend material meeting the above preferred conditions, for example, NE41 (trade name: 40 parts by weight, EPDM: 60 parts by weight, HAF carbon: 5 parts by weight, manufactured by JSR Corporation) 5 parts by weight of Zn0),
"NE61" (60 parts by weight of NBR, 40 parts by weight of EPDM, 5 parts by weight of HAF carbon, 5 parts by weight of Zn0),
"NE71" (70 parts by weight of NBR, 30 parts by weight of EPDM, 5 parts by weight of HAF carbon, 5 parts by weight of Zn0) and the like.

[Ingredients] As the above-mentioned organic peroxide,
Those used for so-called peroxide vulcanization can be used without limitation. For example, dicumyl peroxide (D
CP), 1,1-bis (t-butylperoxy) 3,
3,5-trimethylcyclohexane and the like can be exemplified, and as a trade name, "Perhexa 25B" manufactured by NOF Corporation can be exemplified.

As for sulfur or the vulcanization accelerator, both of them may be added, or only one of them may be added. As vulcanization accelerators, those used in sulfur vulcanization systems or peroxide vulcanization systems can be used arbitrarily, and their trade names are all manufactured by Ouchi Shinko Chemical Industry Co., Ltd. "Suncellar CZ", "Noxeller C
Z "," Noxeller TET "," Noxeller D "," Barnock R "manufactured by NOF Corporation," Santogard PVI "manufactured by Mitsubishi Monsanto Kasei Co., Ltd., and the like.

The rubber composition according to the present invention further comprises:
It is preferable to add 1 to 20 parts by weight of the hydrotalcite compound to 100 parts by weight of the blend material. The hydrotalcite compound is a substance having a crystal structure represented by the following general formula “Chemical formula 1”.

[0032]

Embedded image In the above formula, x is a numerical value in the range of 0 <x ≦ 0.33, and M represented by +2 valence is Mg, Mn, Fe, Co,
M, which represents divalent metal ions such as Ni, Cu, Zn, etc. in +3 valence,
Trivalent metal ions such as Al, Fe, Cr, Co, and In are shown. A represented by -n valence is an acetate ion, an oxalate ion, a salicate ion, a monovalent hydroxyl ion, a fluorine ion, a chlorine ion, a bromine ion or a nitrate ion;
A trivalent carbonate ion or a sulfate ion, a trivalent ferricyan ion and the like. [Other Additives] The rubber composition of the present invention may contain, in addition to the above-mentioned various additives, other types of additives that may be added to the rubber composition as long as the functions and effects of the present invention are not impaired. For example, carbon black, a plasticizer, a process oil, a processing aid, an antioxidant and the like can be optionally added.

[Laminate and Hose] In the present invention, the term “laminate” refers to a rubber composition layer using the rubber composition according to the present invention, an acrylic rubber, a nitrile rubber, an epichlorohydrin rubber, and a chlorinated polyethylene rubber. Alternatively, a rubber material layer using a chlorosulfonated polyethylene rubber is laminated and bonded with or without a reinforcing layer, and a laminated body other than a hose is also included. It is not limited to a laminate used for components related to air piping and oil piping.

The type of the acrylic rubber is not limited, but preferred examples thereof include ethylene acrylic rubber and ethylene vinyl acetate rubber. The type of the nitrile rubber is not limited.
-NBR blended with NBR (hydrogenated NBR) and PVC
R and PVC can be preferably exemplified. The type of the epichlorohydrin rubber is not limited, but preferred examples thereof include a homopolymer of epichlorohydrin (CO) and a copolymer of epichlorohydrin-ethylene oxide (ECO). These CO and ECO include:
Includes copolymers of allyl glycidyl ether. The chlorinated polyethylene rubber and the chlorosulfonated polyethylene rubber include various grades having different amounts of chlorine without limitation.

In the present invention, the hose refers to a hose using the above-mentioned laminated body.
For example, air hoses, oil hoses, and the like for automobiles can be cited, but are not necessarily limited to hoses for these uses.

[0036]

Examples ( Compounding of rubber composition) The compounding compositions of Examples 1 to 8 shown in Table 1 at the end, Comparative Examples 1, 2 and 4 shown in Tables 3 and 4 at the end. According to the blending recipe of Example 10 (all the numerical values in the table are expressed in parts by weight), in each example, all components other than the vulcanized system were kneaded with a Banbury mixer, and then the vulcanized compounding agent was added. Kneaded by open roll.

In Tables 1 and 3, "JSR NE4
1 "," JSR NE61 "and" JSR NE71 "are all blended materials having the above-mentioned contents manufactured by JSR Corporation, and" JSR EP22 "is an ESR manufactured by JSR Corporation.
PDM and “JSR N230S” means JSR
This is NBR manufactured by K.K. "Stearic acid" and "Emaster 510P" are processing aids, and among them, "Emaster 510P" is a fatty acid ester manufactured by Riken Vitamin Co., Ltd. "Antiaging agent CD" is an antiaging agent manufactured by Ouchi Shinko Chemical Co., Ltd. Next, "DHT-4
"A" means "Alkamizer 4" manufactured by Kyowa Chemical Co., Ltd.
Are hydrotalcite compounds manufactured by Kyowa Chemical Industry Co., Ltd. "Perhexa 25B" is an organic peroxide manufactured by NOF Corporation, and "Varnock R" is a sulfur-based vulcanizing agent manufactured by NOF Corporation.
"Z" is a vulcanization accelerator manufactured by Ouchi Shinko Chemical Co., Ltd.

In Table 4, "JSR EP35"
Is EPDM manufactured by JSR Corporation, and "Anti-aging agent 3
"C" is an anti-aging agent manufactured by Seiko Chemical Co., Ltd., and "Anti-aging agent AW" and "Anti-aging agent NBC" are anti-aging agents manufactured by Ouchi Shinko Chemical Co., Ltd.

( Material Performance of Rubber Composition ) In order to evaluate the material performance of the rubber composition according to each of the above Examples and Comparative Examples,
The following tests were performed.

A) For the unvulcanized rubber composition according to each example,
Mooney viscosity [ML121 ° C 1 + 3 (poi) under normal conditions and after wet heat treatment (50 ° C × 95% RH × 48 hours)
nt)] and scorch time [St.5p (min)]. The results are shown in Tables 2 to 4 at the end. In the corresponding column in the table, the upper value indicates Mooney viscosity, and the lower value indicates scorch time.

The value of Mooney viscosity is 25 to
It is considered that about 45 is preferable for the scorch time to be 15 minutes or more.

B) For the unvulcanized rubber composition according to each example,
A test piece was prepared by press vulcanization at 160 ° C./45 minutes. And about these test pieces, JIS K6
251 and physical property tests [TB (MPa), EB
(%), Hs (point)]. Next, to evaluate the heat resistance of the test piece, after heat aging at 135 ° C / 72 hours, after heat aging at 135 ° C / 168 hours, and at 135 °
After the heat aging of C / 240 hours, the same physical property test was performed.
The results are shown in the corresponding columns of the above tables, where the upper numerical value is TB, the central numerical value is EB,
The lower numerical value indicates Hs, and in the heat resistance evaluation, TB is expressed as △ TB (%), EB is expressed as △ EB (%), and Hs is expressed as △ Hs (point). ing.

The physical properties under normal conditions were TB of 9.8M.
Pa and EB are preferably 250% or more,
As heat resistance, after heat aging, △ TB, △ EB, △ H
It is considered preferable that s is equivalent to ECO.

C) A vulcanized test piece having a prescribed shape was prepared using the unvulcanized rubber composition according to each example,
The compression set (%) after heat resistance of × 72 hours and after heat resistance of 120 ° C. × 72 hours was evaluated. These results are shown in the corresponding columns of the above tables.

The compression set after heat resistance at 100 ° C. for 72 hours is 40% or less, and the compression set is 120 ° C. × 72.
It is considered that the compression set after the heat resistance for 60 hours is preferably 60% or less.

D) In order to evaluate the oil resistance of the test piece according to each of the above examples, the test piece was immersed in an evaluation oil “IRM903” at 100 ° C. for 72 hours, and the TB, EB, The change in Hs and the volume change were measured. The results are shown in the corresponding columns of the above tables.
(%), The second value is △ EB (%), the third value is △ Hs (point), and the bottom value is the volume change rate △ V
(%). In addition, it is considered that the numerical value of each evaluation item relating to the oil resistance is preferably equal to CR.

E) The test piece according to each of the above examples was subjected to JIS
The embrittlement temperature (° C.) was measured according to K 6261,
The low-temperature embrittlement was evaluated. The results are shown in the corresponding columns of the above tables. It is considered that the embrittlement temperature is preferably −30 ° C. or less.

F) After preparing a 2 mm thick sheet using the unvulcanized rubber composition according to each of the above examples, the sheet was heated at 160 ° C. × 45.
A test piece was prepared by subjecting it to steam vulcanization for one minute. According to JIS K 6259, these test pieces were not subjected to any pretreatment, and were subjected to 0 to 50 pph × 40 ° C.
After extending by 30%, the dynamic ozone property was evaluated. In addition, about dynamic ozone property, O.D. K. Is considered preferable.

(Preparation of Laminate and Peeling Test ) An unvulcanized sheet having a thickness of 1.7 mm using the rubber composition according to the compounding formulation of Example 1 and “Acrylic rubber compounding contents” in Table 6 at the end Of the 1.7 mm thick unvulcanized sheet using an acrylic rubber according to the formulation shown in the section (all numerical values in the table are expressed in parts by weight; the same applies hereinafter).
Example 9 Press vulcanization at 160 ° C for 45 minutes at cm ²
Was produced.

In the same manner as described above, a laminate comprising an unvulcanized sheet of the rubber composition according to the compounding recipe of Example 1 and an unvulcanized sheet of the nitrile rubber according to the compounding recipe of Comparative Example 6 was prepared. Example 10 was performed.

In the same manner as above, the unvulcanized sheet of the rubber composition according to the compounding formulation of Example 1 and “NB” in Table 6 at the end
NB related to the formulation shown in the section “R / PVC material formulation”
A laminate composed of an uncured R / PVC sheet was prepared as Example 11.

In the same manner as above, the unvulcanized sheet of the rubber composition according to the compounding formulation of Example 1 and “H-
H-NB according to the formulation shown in the section “NBR material formulation”
A laminated body composed of an unvulcanized sheet of R (hydrogenated NBR) was prepared as Example 12.

In the same manner as above, a laminate comprising an unvulcanized sheet of the rubber composition according to the compounding formula of Example 1 and an unvulcanized sheet of epichlorohydrin rubber according to the compounding formula of Comparative Example 9 was prepared. Example 13 was performed.

In the same manner as above, the uncured sheet of the rubber composition according to the compounding formulation of Example 1 and “EC
Example 14 was made as a laminate including an unvulcanized sheet of epichlorohydrin-based rubber according to the compounding recipe shown in the section “O material-2 compounding content”.

In the same manner as above, the unvulcanized sheet of the rubber composition according to the compounding formulation of Example 1 and “CP
Example 15 was prepared as a laminate including an unvulcanized sheet of a chlorinated polyethylene rubber according to the formulation shown in the section of “E material formulation”.

In the same manner as above, an unvulcanized sheet of the rubber composition according to the compounding formulation of Example 1 and “CS
Example 16 A laminate comprising a chlorosulfonated polyethylene-based rubber and an unvulcanized sheet according to the formulation shown in the section “M material formulation” was prepared.

The laminates according to Examples 9 to 16 were subjected to a T-type peel test according to JIS K 6256 in an initial state, and a peel strength after curing (kgf / inch).
Was measured. The state of the separated interface was visually observed.

Table 5 shows the results of the T-type peel test of each of the above Examples.
Is shown in the corresponding column. Generally, their peel strength is 4.0.
Although it is considered preferable to be not less than kgf / inch, each of the examples showed a peel strength exceeding 6 kgf / inch. Moreover, the state of the peeling interface is as follows in all the examples.
The state was "partial rubber failure" where partial destruction of the rubber layer was observed at the interface, or "rubber destruction" where destruction of the rubber layer was observed at the entire interface. This confirmed the excellent peel strength by visual observation.

[0059]

[Table 1]

[0060]

[Table 2]

[0061]

[Table 3]

[0062]

[Table 4]

[0063]

[Table 5]

[0064]

[Table 6]

[0065]

[Table 7]

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Claims (8)

[Claims] 1. A nitrile rubber and EPDM (ethylene-
(Propylene-diene terpolymer rubber) and nitrile rubber: EPDM = 100: 30 parts by weight of a blended material blended in a ratio within the range of 70:30 to 40:60 with respect to the following (1) and ( A rubber composition comprising the component (2). (1) Organic peroxide: 0.5 to 10 parts by weight. (2) Sulfur or vulcanization accelerator: 0.3 to 5 parts by weight. 2. The rubber composition further comprises a hydrotalcite compound in an amount of 1 to 100 parts by weight of the blend material.
The rubber composition according to claim 1, wherein 20 parts by weight are added. 3. A rubber composition layer using the rubber composition according to claim 1 or 2 and a rubber material layer using an acrylic rubber with or without a reinforcing layer. A laminate characterized by being laminated and adhered to the laminate. 4. A rubber composition layer using the rubber composition according to claim 1 or 2 and a rubber material layer using a nitrile rubber with or without a reinforcing layer. A laminate characterized by being laminated and adhered to the laminate. 5. A rubber composition layer using the rubber composition according to claim 1 or 2 and a rubber material layer using epichlorohydrin rubber with or without a reinforcing layer. A laminate characterized by being laminated and adhered to the laminate. 6. A rubber composition layer using the rubber composition according to claim 1 or 2 and a rubber material layer using a chlorinated polyethylene rubber via a reinforcing layer or A laminated body characterized by being laminated and bonded without interposition. 7. A rubber composition layer using the rubber composition according to claim 1 or 2 and a rubber material layer using a chlorosulfonated polyethylene rubber via a reinforcing layer. Alternatively, a laminated body characterized by being laminated and adhered without any intervention. 8. A hose using the laminate according to any one of claims 3 to 7.