CN110922690A - Oil-resistant weather-resistant high-air-tightness rubber material and preparation method thereof - Google Patents
Oil-resistant weather-resistant high-air-tightness rubber material and preparation method thereof Download PDFInfo
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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
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
- C08L23/28—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
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Abstract
An oil-resistant weather-resistant high-air-tightness rubber material and a preparation method thereof are disclosed, wherein the rubber material comprises the following substances in parts by weight: 100 parts of a composite material of chlorinated butyl rubber (CIIR) and Chloroprene Rubber (CR), 30-50 parts of a reinforcing agent, 5-20 parts of a nano-grade material, 5-10 parts of active zinc oxide, 2-5 parts of an anti-aging agent, 2-3 parts of a coupling agent, 2-5 parts of a process aid, 5-10 parts of a softening plasticizer, 2-5 parts of an airtight aid and 3-5 parts of an accelerator. The preparation method of the rubber material comprises five steps of nano material premixing treatment, mixing, vulcanizing, cold roll mixing and vulcanizing. The oil-resistant weather-resistant high-air-tightness rubber material prepared by the technical scheme has the advantages of widening the application range of the airtight rubber material, prolonging the service life of airtight rubber products, improving the market competitiveness of the airtight rubber products and having higher economic value due to the oil resistance and weather resistance.
Description
Technical Field
The invention relates to the technical field of rubber composite materials, in particular to a weather-resistant, oil-resistant and high-air-tightness rubber material and a preparation method thereof.
Background
In recent years, the demand for rubber parts for automobiles has increased dramatically due to the increasing production of automobiles. Only automobile rubber tubes (calculated according to the average rubber tube used by each automobile by 20, the minimum requirement of the rubber tubes for the maintenance of new automobiles and old automobiles reaches hundreds of millions of meters in 2019) need thousands of tons of rubber materials, wherein the rubber materials of the inner liner layer account for nearly half of the rubber materials.
At present, the inner liner of the domestic automobile rubber hose is mainly butyl rubber. Although butyl rubber has good air tightness and excellent physical properties, the butyl rubber has poor ozone resistance and oil resistance, and the maximum service temperature is 100 ℃. Along with the improvement of people to the requirement of automobile comfort, the power of engine is bigger and bigger, more and more crowdedly under the engine bonnet, and streamlined design makes air cycle variation again, so that the temperature under the engine bonnet is higher and higher, lead to the rubber tube life of original butyl rubber class to shorten, in addition novel oil gas fuel mixture's application, not only put forward higher requirement on the gas tightness to the automobile rubber tube, and made the requirement to oil resistance, resistant weather ability, original butyl rubber is because resistant oily poor, can not satisfy present rapid development's demand. Oil-resistant and weather-resistant high-air-tightness rubber materials are a trend of market development in the future.
Therefore, it is necessary to develop oil-resistant weather-resistant rubber materials with high air tightness, and great economic and social benefits are certainly generated.
Disclosure of Invention
The invention aims to provide an oil-resistant weather-resistant high-air-tightness rubber material and a preparation method thereof, and aims to solve the problem of poor oil resistance of the existing airtight rubber material.
In order to achieve the purpose, the invention adopts the technical scheme that:
the weather-resistant, oil-resistant and high-air-tightness rubber material is characterized by comprising, by mass, 100 parts of rubber, 30-50 parts of a reinforcing agent, 5-20 parts of a nanoscale material, 5-10 parts of active zinc oxide, 2-5 parts of an anti-aging agent, 2-3 parts of a coupling agent, 2-5 parts of a process aid, 5-10 parts of a softening plasticizer, 2-5 parts of an air-tightness aid and 3-5 parts of an accelerator. The air-tight sealing material also comprises 2-3 parts of an antiozonant NBC and 2-5 parts of an air-tight auxiliary agent; the 100 parts of rubber are composed of 55-75 parts of chlorinated butyl rubber (CIIR) and 25-45 parts of Chloroprene Rubber (CR).
The mass fraction of chlorinated butyl rubber (CIIR) in the matrix rubber in the composite material of chlorinated butyl rubber (CIIR) rubber and Chloroprene Rubber (CR) is at least 55%.
The reinforcing agent filler is one or a mixture of two of fine-particle carbon black and high-mesh light calcium carbonate in any proportion;
the nano material is a mixture of any two or three of nano carbon black, nano silicate, nano oxide and nano calcium carbonate in any proportion.
The coupling agent is any one of silane coupling agent and titanate coupling agent.
The softening plasticizer is any one of high-grade asphalt and environment-friendly oil MESAMOLL or a mixture of two of the high-grade asphalt and the environment-friendly oil MESAMOLL in any proportion.
The antiozonant and the antioxidant are simultaneously NBC and any one of antioxidant 445 or antioxidant MBZ, wherein the antiozonant NBC is not less than 2 parts by weight.
The air-tight auxiliary agent is composed of SD1517, wherein the mass portion is not less than 2.
The accelerator in the vulcanization assistant is a mixture of any two or three of CZ, NOBS, HVA-2 and ZDBC in any proportion.
A preparation method of an oil-resistant weather-resistant high-air-tightness rubber material comprises five steps of nano material pretreatment, mixing, vulcanizing, cold roll mixing and vulcanizing:
(1) pretreatment of the nano material: treating all nano materials with a coupling agent according to the same mass fraction of the formula, adding a certain amount of chloroprene rubber on an open mill, keeping the roller spacing at 0.1mm, keeping the roller temperature at not higher than 40 ℃, thinly passing for 5-6 times, and standing for later use;
(2) mixing: mixing chlorinated butyl rubber and chloroprene rubber in an internal mixer according to a formula ratio, controlling the mixing temperature to be 100-105 ℃, and keeping the mixing time for 3 min; then thinly passing the mixture on an open mill for 4 times; putting the compounded rubber, the anti-aging agent, the antiozonant and the auxiliary agent into an internal mixer, and mixing for 2 min; sequentially adding a reinforcing agent and a plasticizer, mixing for 3min, discharging rubber at the temperature of 110-115 ℃ in an internal mixer, and discharging sheets; standing the mixed rubber for 24 hours for later use;
(3) vulcanizing blended rubber: putting the rubber compound refined in the step 2 into an open mill for hot refining until the rubber compound is smooth, adding active zinc oxide and an accelerator, keeping the roller spacing of 0.1mm after the active oxidizability and the accelerator are completely consumed, passing through for 3 times, and packaging in triangular bags for 3 times; left and right turning and tamping for 6 times, and standing the lower piece for 12 h;
(4) adding the nano material premix and the blended rubber, and mixing on a cold roll on an open mill: and c, keeping the distance between the rollers to be 0.1mm, keeping the roller temperature to be lower than 40 ℃, passing through the rollers for 4-6 times in a thin mode, and turning and tamping the rollers for 4-6 times left and right on an open mill to obtain the oil-resistant and ozone-resistant high-air-tightness rubber material.
(5) And (3) vulcanization: and standing for 24 hours, then, remilling the rubber compound obtained in the test out of pieces, putting the pieces into a mold, and vulcanizing on a flat vulcanizing machine for 25-35 min at the vulcanization temperature of 150-160 ℃ and under the vulcanization pressure of 10-15 MPa.
Compared with the prior art, the scheme has the following advantages and effects:
1. the invention solves the problem that the traditional airtight rubber material is not oil gas resistant, so that the airtight rubber product can be used for a long time in the environment with oil gas.
2. The invention widens the application range and the service life of the airtight rubber material, can be applied to the environment with oil and gas under the condition of excellent airtightness, not only can be used for automobile rubber hoses, but also can be used in rubber products requiring airtightness, such as oil and gas fields and the like.
3. The oil-resistant weather-resistant high-air-tightness rubber material disclosed by the invention has excellent comprehensive performance, good elasticity and mechanical properties, good adhesion performance with a metal part, good fluidity and other excellent processing performances.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
The formula is selected from 80g of chlorinated butyl rubber, 20g of low-crystallinity chloroprene rubber, 5g of nano zinc oxide, 15g of N220 carbon black, 20g of N330 carbon black, 10g of nano carbon black, 5g of active zinc oxide, 3g of anti-aging agent NBC, 4451.5 g of anti-aging agent, 3 parts of coupling agent, g, 10g of environment-friendly plasticizer, 2g of airtight auxiliary agent, 1g of accelerator ZDBC, 1.5g of accelerator NOBS and 22 g of accelerator HVA-22.
a. Pretreatment of the nano material: after 5g of nano zinc oxide and 10g of nano carbon black are treated by a titanate coupling agent according to the same mass fraction, 10g of chloroprene rubber is added on an open mill, the roller spacing is kept at 0.1mm, the roller temperature is kept at 25-40 ℃, and the thin passing is carried out for 5-6 times;
b. banburying and blending chlorinated butyl rubber and chloroprene rubber: mixing chlorinated butyl rubber and chloroprene rubber in an internal mixer according to a formula ratio, controlling the mixing temperature to be 100-110 ℃, and keeping the mixing time for 3 min; then thinly passing the mixture on an open mill for 4 times; putting the compounded rubber, the anti-aging agent, the antiozonant and the auxiliary agent into an internal mixer, and mixing for 2 min; sequentially adding a reinforcing agent and a plasticizer, mixing for 3min, discharging rubber at the temperature of 110-115 ℃ in an internal mixer, and discharging sheets; standing the mixed rubber for 24 hours for later use;
c. vulcanizing blended rubber: b, putting the rubber compound refined in the step b into an open mill for hot refining until the rubber compound is smooth, adding active zinc oxide and an accelerator, keeping the roller spacing of 0.1mm after the active oxidizability and the accelerator are completely consumed, passing through for 3 times, and packaging in triangular bags for 3 times; left and right turning and tamping for 6 times, and standing the lower piece for 12 h;
d. adding the nano material premix and the blended rubber, and mixing on a cold roll on an open mill: and c, keeping the distance between the rollers to be 0.1mm, keeping the roller temperature to be lower than 40 ℃, passing through the rollers for 4-6 times in a thin mode, and turning and tamping the rollers for 4-6 times left and right on an open mill to obtain the oil-resistant and ozone-resistant high-air-tightness rubber material.
And (3) putting the rubber compound obtained in the test into a mold, and vulcanizing on a flat vulcanizing machine for 25min at the vulcanization temperature of 155 ℃ and the vulcanization pressure of 13 +/-1 MPa to prepare the material sample. The results of hardness, tensile strength, elongation at break, oil resistance and air permeability of the obtained rubber material are detected according to national standards and are shown in table 1.
Example 2
The formula is selected from 70g of chlorinated butyl rubber, 30g of low-crystallinity chloroprene rubber, 5g of nano zinc oxide, 20g of N220 carbon black, 10g of nano calcium carbonate, 5g of nano carbon black, 6g of active zinc oxide, 3g of anti-aging agent NBC, 1.5g of anti-aging agent MBZ, 4g of coupling agent, 2g of process auxiliary agent, 10g of environment-friendly plasticizer, 2g of airtight auxiliary agent, 1.5g of accelerator ZDBC, 1.5g of accelerator NOBS and 22 g of accelerator HVA.
a. Pretreatment of the nano material: treating 6g of nano zinc oxide, 5g of nano carbon black and 10g of nano calcium carbonate by using a silane coupling agent according to the same mass fraction, adding 10g of chloroprene rubber on an open mill, keeping the roller spacing of 0.1mm, keeping the roller temperature at about 40 ℃, and passing for 6 times;
b. mixing chlorinated butyl rubber and chloroprene rubber: mixing chlorinated butyl rubber and chloroprene rubber in an internal mixer according to a formula ratio, controlling the mixing temperature to be 100-105 ℃, and keeping the mixing time for 3 min; then thinly passing the mixture on an open mill for 4 times; putting the compounded rubber, the anti-aging agent, the antiozonant and the auxiliary agent into an internal mixer, and mixing for 2 min; sequentially adding a reinforcing agent and a plasticizer, mixing for 3min, discharging rubber at the temperature of 110-115 ℃ in an internal mixer, and discharging sheets; standing the mixed rubber for 24 hours for later use;
c. vulcanizing blended rubber: b, putting the rubber compound refined in the step b into an open mill for hot refining until the rubber compound is smooth, adding active zinc oxide and an accelerator, keeping the roller spacing of 0.1mm after the active oxidizability and the accelerator are completely consumed, passing through for 3 times, and packaging in triangular bags for 3 times; left and right turning and tamping for 6 times, and standing the lower piece for 12h for later use;
d. adding the nano material premix and the blended rubber, and mixing on a cold roll on an open mill: and c, keeping the distance between the rollers to be 0.1mm, keeping the roller temperature to be lower than 40 ℃, passing through the rollers for 4-6 times in a thin mode, and turning and tamping the rollers for 4-6 times left and right on an open mill to obtain the oil-resistant and ozone-resistant high-air-tightness rubber material.
And (3) putting the rubber compound obtained in the test into a mold, and vulcanizing on a flat vulcanizing machine for 15min at the vulcanization temperature of 155 ℃ and the vulcanization pressure of 12 +/-1 MPa to obtain the graphene composite damping rubber material. The results of testing the hardness, tensile strength, elongation at break, oil resistance and air permeability of the obtained rubber material according to the national standards are shown in Table 2.
Example 3
The formula is prepared from 55g of chlorinated butyl rubber, 45g of low-crystallinity chloroprene rubber, 10g of nano zinc oxide, 35g of N220 carbon black, 10g of nano carbon black, 10g of active zinc oxide, 3g of anti-aging agent NBC, 4452.5 g of anti-aging agent, 3 parts of coupling agent, g of environment-friendly plasticizer, 3g of airtight auxiliary agent, 1.5g of accelerator ZDBC, 1.5g of accelerator CZ and 22 g of accelerator HVA-22.
a. Pretreatment of the nano material: after 10g of nano zinc oxide and 10g of nano carbon black are treated by a silane coupling agent according to the same mass fraction, 10g of chloroprene rubber is added on an open mill, the roller spacing is kept at 0.1mm, the roller temperature is kept at about 40 ℃, and the mixture is passed through for 6 times;
b. mixing chlorinated butyl rubber and chloroprene rubber: mixing chlorinated butyl rubber and chloroprene rubber in an internal mixer according to a formula ratio, controlling the mixing temperature to be 100-105 ℃, and keeping the mixing time for 3 min; then thinly passing the mixture on an open mill for 4 times; putting the compounded rubber, the anti-aging agent, the antiozonant and the auxiliary agent into an internal mixer, and mixing for 2 min; sequentially adding a reinforcing agent and a plasticizer, mixing for 3min, discharging rubber at the temperature of 110-115 ℃ in an internal mixer, and discharging sheets; standing the mixed rubber for 24 hours for later use;
c. vulcanizing blended rubber: b, putting the rubber compound refined in the step b into an open mill for hot milling until the rubber compound is smooth,
adding active zinc oxide and an accelerant, keeping the roller spacing of 0.1mm after the feeding of the active zinc oxide and the accelerant is finished, passing through the roller for 3 times, and packaging in triangular bags for 3 times; left and right turning and tamping for 6 times, and standing the lower piece for 12h for later use;
d. adding the nano material premix and the blended rubber, and mixing on a cold roll on an open mill: and c, keeping the distance between the rollers to be 0.1mm, keeping the roller temperature to be lower than 50 ℃, passing through the rollers for 4-6 times in a thin mode, and turning and tamping the rollers for 4-6 times left and right on an open mill to obtain the oil-resistant and ozone-resistant high-air-tightness rubber material.
And (3) putting the rubber compound obtained in the test into a mold, and vulcanizing on a flat vulcanizing machine for 15min at the vulcanization temperature of 155 ℃ and the vulcanization pressure of 12 +/-1 MPa to obtain the graphene composite damping rubber material. The results of testing the hardness, tensile strength, elongation at break, oil resistance and air permeability of the obtained rubber material according to the national standards are shown in Table 3.
In a word, the invention provides the oil-resistant weather-resistant high-air-tightness rubber material and the preparation method thereof, the implementation process is simple and easy, and the industrial value is better. It should be noted that the invention provides many different ideas and methods for implementing the same, and the above-mentioned embodiments are only preferred embodiments of the invention, and the invention is not limited to the above-mentioned embodiments, and equivalent modifications to the invention are also within the scope of the invention.
Claims (10)
1. A weather-resistant, oil-resistant and high-air-tightness rubber material is characterized by comprising, by mass, 100 parts of rubber, 30-50 parts of a reinforcing agent, 5-20 parts of a nanoscale material, 5-10 parts of active zinc oxide, 2-5 parts of an anti-aging agent, 2-3 parts of a coupling agent, 2-5 parts of a process auxiliary agent, 5-10 parts of a softening plasticizer, 2-5 parts of an air-tightness auxiliary agent and 3-5 parts of an accelerator;
the air-tight sealing material also comprises 2-3 parts of an antiozonant NBC and 2-5 parts of an air-tight auxiliary agent; the 100 parts of rubber are composed of 55-75 parts of chlorinated butyl rubber (CIIR) and 25-45 parts of Chloroprene Rubber (CR).
2. An oil-resistant, weather-resistant, and high-airtightness rubber material according to claim 1, wherein the mass fraction of the chlorinated butyl rubber (CIIR) rubber in the matrix rubber in the composite of chlorinated butyl rubber (CIIR) rubber and Chloroprene Rubber (CR) is at least 55%.
3. The oil-resistant weather-resistant high-airtightness rubber material as claimed in claim 1, wherein: the reinforcing agent filler is one or a mixture of two of fine-particle carbon black and high-mesh light calcium carbonate in any proportion.
4. The oil-resistant weather-resistant high-airtightness rubber material as claimed in claim 1, wherein: the nano material is a mixture of any two or three of nano carbon black, nano silicate, nano oxide and nano calcium carbonate in any proportion.
5. The oil-resistant weather-resistant high-airtightness rubber material as claimed in claim 1, wherein: the coupling agent is any one of silane coupling agent and titanate coupling agent.
6. The oil-resistant weather-resistant high-airtightness rubber material as claimed in claim 1, wherein: the softening plasticizer is any one of high-grade asphalt and environment-friendly oil MESAMOLL or a mixture of two of the high-grade asphalt and the environment-friendly oil MESAMOLL in any proportion.
7. The oil-resistant weather-resistant high-airtightness rubber material as claimed in claim 1, wherein: the antiozonant and the antioxidant are simultaneously NBC and any one of antioxidant 445 or antioxidant MBZ, wherein the antiozonant NBC is not less than 2 parts by weight.
8. The oil-resistant weather-resistant high-airtightness rubber material as claimed in claim 1, wherein: the air-tight auxiliary agent is composed of SD1517, wherein the mass portion is not less than 2.
9. The oil-resistant weather-resistant high-airtightness rubber material as claimed in claim 1, wherein: the accelerator in the vulcanization assistant is a mixture of any two or three of CZ, NOBS, HVA-2 and ZDBC in any proportion.
10. A preparation method of an oil-resistant weather-resistant high-air-tightness rubber material is characterized by comprising five steps of nano material pretreatment, mixing, vulcanizing, cold roll mixing and vulcanizing:
(1) pretreatment of the nano material: treating all nano materials with a coupling agent according to the same mass fraction of the formula, adding a certain amount of chloroprene rubber on an open mill, keeping the roller spacing at 0.1mm, keeping the roller temperature at not higher than 40 ℃, thinly passing for 5-6 times, and standing for later use;
(2) mixing: mixing chlorinated butyl rubber and chloroprene rubber in an internal mixer according to a formula ratio, controlling the mixing temperature to be 100-105 ℃, and keeping the mixing time for 3 min; then thinly passing the mixture on an open mill for 4 times; putting the compounded rubber, the anti-aging agent, the antiozonant and the auxiliary agent into an internal mixer, and mixing for 2 min; sequentially adding a reinforcing agent and a plasticizer, mixing for 3min, discharging rubber at the temperature of 110-115 ℃ in an internal mixer, and discharging sheets; standing the mixed rubber for 24 hours for later use;
(3) vulcanizing blended rubber: putting the rubber compound refined in the step 2 into an open mill for hot refining until the rubber compound is smooth, adding active zinc oxide and an accelerator, keeping the roller spacing of 0.1mm after the active oxidizability and the accelerator are completely consumed, passing through for 3 times, and packaging in triangular bags for 3 times; left and right turning and tamping for 6 times, and standing the lower piece for 12 h;
(4) adding the nano material premix and the blended rubber, and mixing on a cold roll on an open mill: c, keeping the distance between the rollers to be 0.1mm, keeping the temperature of the rollers to be lower than 40 ℃, passing the rollers through the mixture for 4-6 times, and turning and tamping the mixture for 4-6 times on a left side and a right side on an open mill to obtain the oil-resistant and ozone-resistant high-air-tightness rubber material;
(5) and (3) vulcanization: and standing for 24 hours, then, remilling the rubber compound obtained in the test out of pieces, putting the pieces into a mold, and vulcanizing on a flat vulcanizing machine for 25-35 min at the vulcanization temperature of 150-160 ℃ and under the vulcanization pressure of 10-15 MPa.
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