CN114230945B - Compounding method of fluororubber, nitrile rubber and butyl rubber - Google Patents
Compounding method of fluororubber, nitrile rubber and butyl rubber Download PDFInfo
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- CN114230945B CN114230945B CN202111625908.8A CN202111625908A CN114230945B CN 114230945 B CN114230945 B CN 114230945B CN 202111625908 A CN202111625908 A CN 202111625908A CN 114230945 B CN114230945 B CN 114230945B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/02—Copolymers with acrylonitrile
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
Abstract
The invention provides a compounding method of fluororubber, nitrile rubber and butyl rubber, belonging to the technical field of rubber compounding. According to the invention, the tetrabutyl benzotriazole salt is added into the mixed nitrile rubber as the middle layer, so that the nitrile rubber and the fluororubber can be bonded together during vulcanization. During vulcanization, a contact layer of the nitrile rubber and the fluororubber forms a cross-linked net structure, the bonding strength of the nitrile rubber and the fluororubber is enhanced, the three rubbers are tightly bonded through co-vulcanization, and the use of various adhesives can be reduced. Meanwhile, the performances of the three rubbers are complemented, and the prepared rubber sheet can have the chemical medium resistance of fluororubber, the oil resistance of nitrile rubber and the air tightness of butyl rubber.
Description
Technical Field
The invention relates to the technical field of rubber compounding, in particular to a compounding method of fluororubber, nitrile rubber and butyl rubber.
Background
The butyl rubber is formed by polymerizing isobutene and a small amount of isoprene, has good air tightness and sunlight ozone resistance, and does not resist partial chemical media.
Nitrile rubber is a copolymer obtained by emulsion polymerization of butadiene and acrylonitrile. The oil resistance, the thermal-oxidative aging resistance, the cold resistance and the like of the composite material are good, but the composite material does not resist strong oxidative acid and has poor ozone resistance.
Fluororubbers are synthetic polymer elastomers containing fluorine atoms in the carbon atoms of the main chain or side chains. The material has strong chemical medium resistance, good high-temperature resistance, poor low-temperature resistance and poor chemical medium resistance to partial chemical media.
The three rubbers have complementary properties, and the three rubbers need to be compounded in order to exert the advantages of the three rubbers, but the three rubbers have poor compatibility, and the rubber layer can fall off and separate during compounding under normal conditions.
Disclosure of Invention
The invention aims to provide a compounding method of fluororubber, nitrile rubber and butyl rubber, which can solve the problem of poor compatibility of the three rubbers.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a compounding method of fluororubber, nitrile rubber and butyl rubber, which comprises the following steps:
plasticating raw fluororubber, raw nitrile butadiene rubber and raw butyl rubber to obtain plasticated fluororubber, plasticated nitrile butadiene rubber and plasticated butyl rubber;
mixing the plasticated fluororubber to obtain mixed fluororubber;
mixing the plasticated nitrile-butadiene rubber to obtain mixed nitrile-butadiene rubber; adding tetrabutyl benzotriazole salt into the plasticated nitrile rubber in the mixing process;
mixing the plasticated butyl rubber to obtain mixed butyl rubber;
respectively pre-vulcanizing the mixed fluororubber, the mixed nitrile rubber and the mixed butyl rubber to obtain pre-vulcanized fluororubber, pre-vulcanized nitrile rubber and pre-vulcanized butyl rubber;
and sequentially laminating the pre-vulcanized fluororubber, the pre-vulcanized nitrile rubber and the pre-vulcanized butyl rubber, and putting the laminated layers into a mold for co-vulcanization.
Preferably, the mixing raw materials of the plasticated fluororubber comprise, by mass: 100 parts of plasticated fluororubber, 1-3 parts of dipenta-vulcanizing agent, 2-5 parts of magnesium oxide and 1-3 parts of isocyano triallyl urate.
Preferably, the mixing raw materials of the plasticated nitrile rubber comprise, by mass: 100 parts of plasticated nitrile rubber, 1-3 parts of sulfur, 2-5 parts of zinc oxide, 1-3 parts of accelerator NS, 1-3 parts of stearic acid and 5-10 parts of tetrabutylbenzotriazole salt.
Preferably, the mixing raw materials of the plasticated butyl rubber comprise, by mass: 100 parts of plasticated butyl rubber, 1-2 parts of sulfur, 0.1-0.3 part of magnesium oxide, 1-3 parts of accelerator DM, 1-2 parts of zinc oxide, 1-30 parts of carbon black N66010 and 1-2 parts of stearic acid.
Preferably, the pre-vulcanization temperature of the mixed fluororubber is 140-145 ℃, and the pre-vulcanization time is 20-30 minutes.
Preferably, the pre-vulcanization temperature of the mixed nitrile rubber is 140-145 ℃, and the pre-vulcanization time is 5-10 minutes.
Preferably, the precuring temperature of the mixed butyl rubber is 140-145 ℃, and the precuring time is 10-15 minutes.
Preferably, the temperature of the co-vulcanization is 140-160 ℃ and the time is 10-30 minutes.
Preferably, the mixing of the masticated fluororubber, the masticated butyl rubber and the masticated nitrile rubber is carried out in an open mill, and the roll speeds for mixing the masticated fluororubber, the masticated butyl rubber and the masticated nitrile rubber are independently 20 to 60rpm.
Preferably, the plastication time of the fluororubber is 2 to 3 minutes; the plastication time of the nitrile rubber is 5-10 minutes; the plastication time of the butyl rubber is 2-3 minutes.
The invention provides a method for compounding fluororubber, nitrile rubber and butyl rubber, which comprises the following steps: plasticating raw fluororubber, raw nitrile butadiene rubber and raw butyl rubber to obtain plasticated fluororubber, plasticated nitrile butadiene rubber and plasticated butyl rubber; mixing the plasticated fluororubber to obtain mixed fluororubber; mixing the plasticated nitrile-butadiene rubber to obtain mixed nitrile-butadiene rubber; adding tetrabutyl benzotriazole salt into the plasticated nitrile rubber in the mixing process; mixing the plasticated butyl rubber to obtain mixed butyl rubber; pre-vulcanizing the mixed fluororubber, the mixed nitrile rubber and the mixed butyl rubber respectively to obtain pre-vulcanized fluororubber, pre-vulcanized nitrile rubber and pre-vulcanized butyl rubber; and sequentially laminating the pre-vulcanized fluororubber, the pre-vulcanized nitrile rubber and the pre-vulcanized butyl rubber, and putting the laminated layers into a mould for co-vulcanization.
According to the invention, the tetrabutyl benzotriazole salt is added into the mixed nitrile rubber serving as the middle layer, so that the nitrile rubber and the fluororubber can be bonded together during vulcanization. During vulcanization, the contact layer of the nitrile rubber and the fluororubber can form a cross-linked net structure, so that the bonding strength of the nitrile rubber and the fluororubber is enhanced, the three rubbers are tightly bonded through co-vulcanization, and the use of various adhesives can be reduced. Meanwhile, the performances of the three rubbers are complemented, and the prepared rubber sheet can have the chemical medium resistance of fluororubber, the oil resistance of nitrile rubber and the air tightness of butyl rubber.
Drawings
FIG. 1 is a schematic cross-sectional view of a composite three-layer film according to the present invention; wherein: a 1-butyl rubber layer; 2-a nitrile rubber layer; 3-fluororubber layer.
Detailed Description
The invention provides a method for compounding fluororubber, nitrile rubber and butyl rubber, which comprises the following steps:
plasticating raw fluororubber, raw nitrile rubber and raw butyl rubber to obtain plasticated fluororubber, plasticated nitrile rubber and plasticated butyl rubber;
mixing the plasticated fluororubber to obtain mixed fluororubber;
mixing the plasticated nitrile rubber to obtain mixed nitrile rubber; adding tetrabutyl benzotriazole salt into the plasticated nitrile rubber in the mixing process;
mixing the plasticated butyl rubber to obtain mixed butyl rubber;
pre-vulcanizing the mixed fluororubber, the mixed nitrile rubber and the mixed butyl rubber respectively to obtain pre-vulcanized fluororubber, pre-vulcanized nitrile rubber and pre-vulcanized butyl rubber;
and sequentially laminating the pre-vulcanized fluororubber, the pre-vulcanized nitrile rubber and the pre-vulcanized butyl rubber, and putting the laminated layers into a mould for co-vulcanization.
The invention plasticates raw fluororubber, raw nitrile butadiene rubber and raw butyl rubber respectively to obtain plasticated fluororubber, plasticated nitrile butadiene rubber and plasticated butyl rubber.
In the invention, the plastication time of the raw fluororubber is preferably 2 to 3 minutes; the plastication time of the nitrile rubber is preferably 5 to 10 minutes; the plastication time of the butyl rubber is preferably 2 to 3 minutes. In the invention, the plastication temperature of the raw fluororubber, the raw nitrile rubber and the raw butyl rubber is independently preferably 20-40 ℃.
After obtaining the plasticated fluororubber, the plasticated nitrile rubber and the plasticated butyl rubber, the invention mixes the plasticated rubbers.
The plasticated fluororubber is mixed to obtain the mixed fluororubber. In the present invention, the raw materials for mixing the plasticated fluororubber preferably include, in parts by mass: 100 parts of plasticated fluororubber, 1 to 3 parts of dipenta-vulcanizing agent, 2 to 5 parts of magnesium oxide and 1 to 3 parts of isocyano triallyl urate (TAIC); further, the bis-penta vulcanizing agent is more preferably 1.5 to 2.5 parts; the magnesium oxide is more preferably 3 to 4 parts; the triallyl isocyanurate is more preferably 1.5 to 2.5 parts.
Mixing the plasticated nitrile rubber to obtain mixed nitrile rubber; the method is characterized in that tetrabutyl benzotriazole salt is added into the plasticated nitrile rubber in the mixing process.
In the invention, the mixing raw materials of the plasticated nitrile rubber preferably comprise, by mass: 100 parts of plasticated nitrile rubber, 1-3 parts of sulfur, 2-5 parts of zinc oxide, 1-3 parts of accelerator NS, 1-3 parts of stearic acid and 5-10 parts of tetrabutylbenzotriazole salt. Further, the preferable amount of the sulfur is 1.5-2.5 parts, the amount of the zinc oxide is 3-4 parts, the amount of the accelerator NS is 1.5-2.5 parts, the amount of the stearic acid is 1.5-2.5 parts, and the amount of the tetrabutylbenzotriazole salt (Psalt) is 6-8 parts.
The plasticated butyl rubber is mixed to obtain the mixed butyl rubber.
In the present invention, the mixing raw materials of the plasticated butyl rubber preferably include, in parts by mass: 100 portions of plasticated butyl rubber, 1 to 2 portions of sulfur, 0.1 to 0.3 portion of magnesium oxide, 1 to 3 portions of accelerator DM, 1 to 2 portions of zinc oxide, 1 to 30 portions of carbon black N66010 and 1 to 2 portions of stearic acid. Further, 1.2-1.7 parts of sulfur, 0.15-0.25 part of magnesium oxide, 1.5-2.5 parts of accelerator DM, 1.3-1.7 parts of zinc oxide, 15-25 parts of carbon black N660 and 1.3-1.8 parts of stearic acid.
In the present invention, the mixing of the masticated fluororubber, the masticated butyl rubber and the masticated nitrile rubber is preferably performed in an open mill, and the roll speed for mixing the masticated fluororubber, the masticated butyl rubber and the masticated nitrile rubber is independently preferably 20 to 60rpm.
In the invention, the mass parts of the plasticated fluororubber, the plasticated butyl rubber and the plasticated nitrile rubber are the same.
After the mixed fluororubber, the mixed nitrile rubber and the mixed butyl rubber are obtained, the mixed fluororubber, the mixed nitrile rubber and the mixed butyl rubber are respectively subjected to pre-vulcanization to obtain pre-vulcanized fluororubber, pre-vulcanized nitrile rubber and pre-vulcanized butyl rubber.
In the invention, the pre-vulcanization temperature of the mixed fluororubber is preferably 140-145 ℃, and the pre-vulcanization time is preferably 20-30 minutes; the pre-vulcanization temperature of the mixed nitrile rubber is preferably 140-145 ℃, and the pre-vulcanization time is preferably 5-10 minutes; the pre-vulcanization temperature of the mixed butyl rubber is preferably 140-145 ℃, and the pre-vulcanization time is preferably 10-15 minutes. The invention respectively carries out pre-vulcanization to prevent three layers of rubber from being obviously layered and mixing the rubber when the three layers of rubber are vulcanized together.
After obtaining the pre-vulcanized fluororubber, the pre-vulcanized nitrile rubber and the pre-vulcanized butyl rubber, the pre-vulcanized fluororubber, the pre-vulcanized nitrile rubber and the pre-vulcanized butyl rubber are sequentially laminated and put into a mould for co-vulcanization.
The invention has no special requirements on the thickness of the pre-vulcanized fluororubber, the pre-vulcanized nitrile rubber and the pre-vulcanized butyl rubber, and the thickness can be adjusted by the technical personnel in the field according to the actual requirements.
The invention has no special requirements on the size of the die, and the skilled person can select the die according to the actual needs. In the embodiment of the invention, the thickness of the die is 2mm, and the length and width dimensions are 14cm × 12cm.
In the present invention, the temperature of the co-vulcanization is preferably 140 to 160 ℃, more preferably 150 to 160 ℃, and the time is preferably 10 to 30 minutes, more preferably 15 to 25 minutes.
According to the invention, the tetrabutyl benzotriazole salt is added into the mixed nitrile rubber serving as the middle layer, so that the nitrile rubber and the fluororubber can be bonded together during vulcanization. During vulcanization, the contact layer of the nitrile rubber and the fluororubber can form a cross-linked net structure, so that the bonding strength of the nitrile rubber and the fluororubber is enhanced, the three rubbers are tightly bonded through co-vulcanization, and the use of various adhesives can be reduced.
In the invention, the structure of the composite film obtained by sequentially laminating and vulcanizing the pre-vulcanized fluororubber, the pre-vulcanized nitrile rubber and the pre-vulcanized butyl rubber is shown as figure 1, namely a 1-butyl rubber layer; 2-a nitrile rubber layer; 3-fluororubber layer.
The compounding method of fluororubber, nitrile rubber and butyl rubber provided by the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
1) Plasticating: and respectively feeding raw fluororubber, raw nitrile rubber and raw butyl rubber into an open mill, and setting the temperature to be 40 ℃, wherein the raw butyl rubber and the raw fluororubber need to be plasticated for 3 minutes, and the raw nitrile rubber needs to be plasticated for 10 minutes, so as to obtain plasticated fluororubber, plasticated nitrile rubber and plasticated butyl rubber.
2) Mixing: the plasticated fluororubber, the plasticated nitrile rubber and the plasticated butyl rubber are mixed according to the formula shown in the table 1, and various auxiliaries are added to enable the mixed rubber to meet the performance requirements.
Table 1 example 1 rubber compound formulation
3) Pre-vulcanization and vulcanization: the compounded fluororubber, the compounded nitrile rubber and the compounded butyl rubber were each presulfurized in a vulcanizer using a mold of 14cm × 12cm with a thickness of 1mm at a temperature of 140 ℃, for 10 minutes for the compounded butyl rubber, for 5 minutes for the compounded nitrile rubber and for 20 minutes for the compounded fluororubber. Then cooling the mixture to room temperature, combining the mixture according to the sequence of fluororubber-nitrile rubber-butyl rubber, and finally putting the mixture into a mould with the thickness of 2mm and the thickness of 14cm multiplied by 12cm for vulcanizing 15 minutes at 160 ℃ to obtain a finished product of the compound rubber.
The adhesive-to-adhesive bond strengths obtained using the formulation of example 1 are shown in table 2. The method for testing the adhesive strength is GB/T532-2008.
Table 2 adhesion strength between rubbers of example 1
| Fluororubber and nitrile rubber | Nitrile rubber and butyl rubber | |
| Adhesive strength kN/m between sizing materials | ＞0.99 | ＞0.5 |
Since the prepared film having a high adhesive strength could not be peeled off for testing the adhesive strength. Therefore, only three-layer structures with poor composite conditions can be selected for testing. The adhesion strength of the other samples is greater than the data in table 2, so the adhesion strength in table 2 gives the lower limit.
Comparative example 1
The only difference from example 1 is that the mix formulation is shown in table 3.
TABLE 3 formulation of comparative example 1 rubber compound
The adhesive-to-adhesive bond strengths obtained using the formulation of comparative example 1 are shown in table 4.
TABLE 4 adhesive strength between rubbers of comparative example 1
| Fluororubber and nitrile rubber | Nitrile rubber and butyl rubber | |
| Adhesive strength kN/m between sizing materials | 0 | ＞0.3 |
As can be seen from the above examples and comparative examples, the present invention enhances the adhesive strength between nitrile rubber and fluororubber by adding tetrabutyl benzotriazole salt to the compounded nitrile rubber as an intermediate layer, thereby enabling the nitrile rubber and the fluororubber to be bonded together during vulcanization.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A compounding method of fluororubber, nitrile rubber and butyl rubber is characterized by comprising the following steps:
plasticating raw fluororubber, raw nitrile butadiene rubber and raw butyl rubber to obtain plasticated fluororubber, plasticated nitrile butadiene rubber and plasticated butyl rubber;
mixing the plasticated fluororubber to obtain mixed fluororubber; the plasticated fluororubber comprises the following mixing raw materials in parts by weight: 100 parts of plasticated fluororubber, 1-3 parts of dipenta-vulcanizing agent, 2-5 parts of magnesium oxide and 1-3 parts of isocyano triallyl urate;
mixing the plasticated nitrile rubber to obtain mixed nitrile rubber; adding tetrabutyl benzotriazole salt into the plasticated nitrile rubber in the mixing process; the mixing raw materials of the plasticated nitrile butadiene rubber are as follows by mass: 100 parts of plasticated nitrile rubber, 1-3 parts of sulfur, 2-5 parts of zinc oxide, 1-3 parts of accelerator NS, 1-3 parts of stearic acid and 5-10 parts of tetrabutylbenzotriazole salt;
mixing the plasticated butyl rubber to obtain mixed butyl rubber;
respectively pre-vulcanizing the mixed fluororubber, the mixed nitrile rubber and the mixed butyl rubber to obtain pre-vulcanized fluororubber, pre-vulcanized nitrile rubber and pre-vulcanized butyl rubber;
and sequentially laminating the pre-vulcanized fluororubber, the pre-vulcanized nitrile rubber and the pre-vulcanized butyl rubber, and putting the laminated layers into a mold for co-vulcanization.
2. The compounding method according to claim 1, wherein the raw materials for mixing the masticated butyl rubber comprise, in parts by mass: 100 parts of plasticated butyl rubber, 1-2 parts of sulfur, 0.1-0.3 part of magnesium oxide, 1-3 parts of accelerator DM, 1-2 parts of zinc oxide, 1-30 parts of carbon black N66010 and 1-2 parts of stearic acid.
3. The compounding method according to claim 1, wherein the temperature of the precuring of the compounded fluororubber is 140 to 145 ℃ and the time of the precuring is 20 to 30 minutes.
4. Compounding process according to claim 1, characterized in that the pre-vulcanization temperature of the compounded nitrile rubber is 140-145 ℃ and the pre-vulcanization time is 5-10 minutes.
5. The compounding method according to claim 1, wherein the pre-vulcanization temperature of the compounded butyl rubber is 140 to 145 ℃ and the pre-vulcanization time is 10 to 15 minutes.
6. The compounding method according to claim 1, wherein the temperature of the co-vulcanization is 140 to 160 ℃ for 10 to 30 minutes.
7. The compounding method according to claim 1, characterized in that the mixing of the masticated fluororubber, masticated butyl rubber and masticated nitrile rubber is carried out in an open mill, the roll speeds of the masticated fluororubber, masticated butyl rubber and masticated nitrile rubber mixing being independently 20 to 60rpm.
8. Compounding process according to claim 1, characterized in that the mastication time of the fluororubber is 2 to 3 minutes; the plastication time of the nitrile rubber is 5-10 minutes; the plastication time of the butyl rubber is 2-3 minutes.
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