CN114456504A - Environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding and preparation method thereof - Google Patents
Environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding and preparation method thereof Download PDFInfo
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- CN114456504A CN114456504A CN202210103830.1A CN202210103830A CN114456504A CN 114456504 A CN114456504 A CN 114456504A CN 202210103830 A CN202210103830 A CN 202210103830A CN 114456504 A CN114456504 A CN 114456504A
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- 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
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
An environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding comprises the following raw materials in parts by weight, based on 100 parts by weight of rubber virgin rubber: 90-105 parts of ethylene propylene diene monomer, 30-40 parts of carbon black N550, 40-50 parts of carbon black N774, 10-20 parts of pottery clay N85, 10-30 parts of polyisobutylene, 2-5 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.6-0.8 part of anti-aging agent SP-P, 1.5-3 parts of peroxide vulcanizing agent BIBP and 5-15 parts of peroxide co-crosslinking agent butadiene rubber BR 9000. The invention can greatly improve the release effect of the EPDM peroxide vulcanization formula without adding auxiliary additives, is suitable for automatic production and can reduce the raw material cost to a certain extent.
Description
Technical Field
The invention relates to the field of rubber, in particular to an environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding and a preparation method thereof.
Background
In the production process of various domestic rubber factories, certain products in the aspect of life are frequently encountered, and sealing products meeting NSF and meeting drinking water or food contact in various countries are needed. Due to the limitations of migration substances, VOC, VOM, oxygen consumption and the like, most of the products need to adopt a peroxide curing system, and a sulfur curing system cannot be used. And EPDM materials adopting peroxide vulcanization have the problems of mold sticking, long vulcanization time and the like. The use of some internal and external release agents is greatly limited because of the concern of drinking water and food. Because of the problem of sticking, the products are difficult to realize automatic production, and the forming efficiency and labor cost cannot be effectively reduced.
At present, DCP (dicumyl peroxide), BIBP (di (tert-butylperoxyisopropyl) benzene), di-penta complex TAC (triallyl cyanurate), TAIC (triallyl isocyanurate), TMPTA (trimethylolpropane triacrylate), TMPTNA (trimethylolpropane trimethacrylate), ZDA (zinc acrylate), ZDMA (zinc dimethacrylate), TRA (dipentamethylenethiuram tetrasulfide) and the like are mostly adopted in domestic EPDM (peroxide vulcanization) systems, and the EPDM peroxide vulcanization systems have advantages and disadvantages in terms of performance. But the complex system can not be comprehensively realized in terms of comprehensive environmental protection and demolding effect. The matching of peroxide, TAC and TAIC has high vulcanization density and good pressure change effect, but automatic demolding cannot be realized. The combination with TMPTA, TMPTNA, ZDA and ZDMA has prominent bonding effect, but is easy to be stuck and has a plurality of troubles in the production of sealing products. The sealing product can be easily detached by matching with TRA, but has overlarge smell, and if the system is used in a drinking water system, flora breeding is easily caused, and the oxygen consumption exceeds the standard. For environment-friendly sealing products, the above systems are not very beneficial, the production efficiency is difficult to improve, and the post-treatment process cost of the products is high. For environment-friendly sealing products, in order to realize effective market competition, the efficiency is improved and the cost is reduced besides the quality of products.
For the EPDM environment-friendly peroxide formula, firstly, because the peroxide vulcanized EPDM material cannot excessively add some auxiliary components due to the environment-friendly requirement (suitable for drinking water), and simultaneously, because the release effect of the peroxide vulcanization is not as good as that of a sulfur vulcanized rubber material, the demoulding of the EPDM peroxide vulcanized product is difficult to become an industrial problem. Meanwhile, because the production management cost and the labor cost are continuously increased, the efficiency is necessarily improved. The need to easily demold the EPDM product to allow for automated production has become a challenge for seal manufacturing enterprises. The scheme is generated.
Disclosure of Invention
The invention aims to provide an environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding and a preparation method thereof, which can greatly improve the release effect of an EPDM peroxide vulcanization formula without adding an auxiliary additive, is suitable for automatic production and can reduce the cost of raw materials to a certain extent.
In order to achieve the above purpose, the solution of the invention is:
an environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding comprises the following raw materials in parts by weight, based on 100 parts by weight of rubber virgin rubber: 90-105 parts of ethylene propylene diene monomer, 30-40 parts of carbon black N550, 40-50 parts of carbon black N774, 10-20 parts of pottery clay N85, 10-30 parts of polyisobutylene, 2-5 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.6-0.8 part of anti-aging agent SP-P, 1.5-3 parts of peroxide vulcanizing agent BIBP and 5-15 parts of peroxide co-crosslinking agent butadiene rubber BR 9000.
Further, the ethylene propylene diene monomer is K2650C of Allandiaceae; the carbon black N550/N774 is SPSO/N774 of cabot; the argil N85 is a Hoffman product N85; the polyisobutylene is H-100 of INEOS; the zinc oxide is AZO-805 of Taiwan diligent; the stearic acid is a product 1801 of Indonesia; the peroxide vulcanizing agent BIBP is PERKADOX 14S-FL; the peroxide auxiliary crosslinking agent butadiene rubber BR9000 is a universal grade butadiene rubber on the market.
Further, 100 parts of ethylene propylene diene monomer, 35 parts of carbon black N550, 45 parts of carbon black N774, 15 parts of pottery clay N85, 15 parts of polyisobutylene, 3 parts of zinc oxide, 0.5 part of stearic acid, 0.7 part of an anti-aging agent SP-P, 2 parts of a peroxide vulcanizing agent BIBP and 10 parts of peroxide co-crosslinking agent butadiene rubber BR 9000.
Further, 100 parts of ethylene propylene diene monomer, 40 parts of carbon black N550, 50 parts of carbon black N774, 20 parts of pottery clay N85, 20 parts of polyisobutylene, 5 parts of zinc oxide, 1 part of stearic acid, 0.8 part of an anti-aging agent SP-P, 3 parts of peroxide curing agent BIBP and 15 parts of peroxide co-crosslinking agent butadiene rubber BR 9000.
The preparation method of the environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding comprises the following raw material components in parts by weight: 90-105 parts of ethylene propylene diene monomer, 30-40 parts of carbon black N550, 40-50 parts of carbon black N774, 10-20 parts of pottery clay N85, 10-30 parts of polyisobutylene, 2-5 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.6-0.8 part of anti-aging agent SP-P, 1.5-3 parts of peroxide vulcanizing agent BIBP and 5-15 parts of peroxide co-crosslinking agent butadiene rubber BR 9000;
the preparation method comprises the following steps:
step 1: firstly, putting ethylene propylene diene monomer and peroxide co-crosslinking agent butadiene rubber BR9000 into an internal mixer, mixing to 80 ℃, then sequentially adding other raw materials except peroxide vulcanizing agent BIBP for mixing, and mixing to about 130 ℃ to obtain uniform master batch;
step 2: after the master batch is kept stand and cooled, adding peroxide vulcanizing agent BIBP according to a proportion, mixing to 85 ℃, discharging, introducing into an open mill, turning over and discharging, and cooling to obtain a final rubber sheet;
and step 3: vulcanizing the final rubber sheet to form a product, and demolding;
and 4, step 4: and the product is subjected to secondary vulcanization at 150 ℃ for 4 hours after being formed.
Furthermore, in the step 1, the mixing temperature is controlled below 130 ℃, and the mixing time is 10-12 minutes.
Further, in the step 2, the master batch and the peroxide vulcanizing agent BIBP are mixed by an open mill or an internal mixer, and the mixing and discharging temperature of the internal mixer is controlled below 85 ℃.
Further, step 3 comprises injection molding or compression molding the final rubber sheet at 182 + -5 ℃ to obtain the product.
Further, in step 3, the final rubber sheet is cut into corresponding strip-shaped rubber materials according to the required specification of the product, and then the strip-shaped rubber materials are molded in a mold at high temperature to form the product.
After the scheme is adopted, the cis-butadiene rubber BR9000 is used as an auxiliary crosslinking agent to replace the traditional auxiliary crosslinking agents TAC \ TAIC \ TMPTA \ TMPAMA \ ZDA \ ZDMA \ TRA, so that the release performance of the EPDM peroxide vulcanized rubber material is improved. The butadiene rubber BR9000 is easy to obtain and low in cost, can reduce part of the cost of the rubber material, and simultaneously avoids the influence of adding other release agents on the environmental protection of the rubber material. The butadiene rubber BR9000 can provide fast free radicals in a peroxide curing system to increase the curing speed of peroxide so as to realize the function of a sizing agent, and the heat resistance and the compression permanent set of the sizing agent are not influenced. Meanwhile, the non-adhesiveness of the butadiene rubber BR9000 is that the EPDM peroxide vulcanized rubber obtains good release property, so that the requirement of automatic production of a company can be met.
Detailed Description
The invention discloses an environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding, which comprises the following raw materials in parts by weight, based on 100 parts by weight of rubber virgin rubber (the rest proportion is relative to the weight of the virgin rubber): 90-105 parts of Ethylene Propylene Diene Monomer (EPDM), 30-40 parts of carbon black N550, 40-50 parts of carbon black N774, 10-20 parts of argil, 10-30 parts of polyisobutylene, 2-5 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.6-0.8 part of antioxidant SP-P, 1.5-3 parts of peroxide vulcanizing agent BIBP (di (tert-butyl peroxyisopropyl) benzene) and 5-15 parts of butadiene rubber BR 9000.
Wherein the EPDM is K2650C of Allandiaceae; the carbon black N550/N774 is SPSO/N774 of Cabot; pottery clay N85 is hoffman product N85; polyisobutylene is H-100 for INEOS; zinc oxide is AZO-805 from tai diligent; stearic acid is Indonesia product 1801; the peroxide vulcanizing agent BIBP is PERKADOX 14S-FL; the peroxide assistant crosslinking agent butadiene rubber BR9000 is a general-purpose grade butadiene rubber on the market.
As the butadiene rubber BR9000 is used as an auxiliary crosslinking agent to replace the traditional auxiliary crosslinking agents TAC \ TAIC \ TMPTA \ TMPAMA \ ZDA \ ZDMA \ TRA, the release performance of the EPDM peroxide vulcanized rubber material can be improved. The butadiene rubber BR9000 is easy to obtain and low in cost, can reduce part of the cost of the rubber material, and simultaneously avoids the influence of adding other release agents on the environmental protection of the rubber material. The butadiene rubber BR9000 can provide fast free radicals in a peroxide curing system to increase the curing speed of peroxide so as to realize the function of a sizing agent, and the heat resistance and the compression permanent set of the sizing agent are not influenced. Compared with other auxiliary crosslinking agents, the butadiene rubber BR9000 serving as the auxiliary crosslinking agent does not increase the content of VOM (volatile organic compound) in the material due to the large molecular weight, so that the requirement of food hygiene is easily met, the low-temperature brittleness of the formula can be improved due to the flexibility of the molecule, the release property and the auxiliary crosslinking property on peroxide are utilized, and the non-adhesiveness of the butadiene rubber BR9000 is that EPDM (ethylene-propylene-diene monomer) peroxide vulcanized rubber obtains good release property, so that the easy demolding is realized, and the requirement of automatic production of a company can be met.
The invention also discloses a preparation method of the environment-friendly peroxide vulcanized EPDM material suitable for automatic demoulding, which comprises the following raw material components in parts by weight: 90-105 parts of ethylene propylene diene monomer, 30-40 parts of carbon black N550, 40-50 parts of carbon black N774, 10-20 parts of pottery clay N85, 10-30 parts of polyisobutylene, 2-5 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.6-0.8 part of anti-aging agent SP-P, 1.5-3 parts of peroxide vulcanizing agent BIBP and 5-15 parts of peroxide co-crosslinking agent butadiene rubber BR 9000. The raw materials are prepared according to the formula proportioning by taking the weight of the rubber virgin rubber as 100 parts.
The preparation method comprises the following steps:
step 1, firstly putting ethylene propylene diene monomer and peroxide co-crosslinking agent butadiene rubber BR9000 into an internal mixer, mixing to 80 ℃, then sequentially adding other raw materials except peroxide vulcanizing agent BIBP for mixing, and mixing to about 130 ℃ to obtain uniform master batch;
step 2: after the master batch is kept stand and cooled, adding a peroxide vulcanizing agent BIBP (1.5-3 parts by weight) according to a proportion, mixing to 85 ℃, discharging, then introducing into an open mill, turning over and mixing to obtain a sheet, and cooling to obtain a final rubber sheet;
and step 3: vulcanizing the final rubber sheet to form a product, and demolding;
and 4, step 4: the formed product was passed through a secondary vulcanization at 150 degrees for 4 hours.
In the step 1, the mixing temperature is controlled below 130 ℃, and the mixing time is 10-12 minutes.
Between step 1 and step 2, the master batch may be allowed to stand for 24 hours for cooling.
In the step 2, the master batch and the peroxide vulcanizing agent BIBP are mixed by an open mill or an internal mixer, and the mixing and discharging temperature of the internal mixer is controlled below 85 ℃.
In the step 3, the step of vulcanizing and molding comprises the step of injection molding or compression molding the final rubber sheet at the temperature of 182 +/-5 ℃ to obtain the product. The final rubber sheet can be cut into corresponding strip rubber according to the required specification of the product, and then the strip rubber is molded into a product (three vulcanization factors, namely mold temperature, molding time and molding pressure) in a mold at high temperature, wherein the molding time is related according to the thickness of the product, and the actual mold test OK condition is used as the standard.
The present invention is illustrated in detail by the following specific examples.
Example 1:
the embodiment 1 of the invention provides an environment-friendly peroxide vulcanized EPDM (ethylene propylene diene monomer) material suitable for automatic demolding, which comprises the following raw materials in parts by weight, calculated by 100 parts by weight of rubber virgin rubber (the rest proportion is relative to the weight of the virgin rubber): 100 parts of ethylene propylene diene monomer, 35 parts of carbon black N55045 parts, N8515 parts of pottery clay, 15 parts of polyisobutene, 3 parts of zinc oxide, 0.5 part of stearic acid, 0.7 part of antioxidant SP-P, 2 parts of peroxide vulcanizing agent BIBP and 900010 parts of peroxide co-crosslinking agent butadiene rubber BR.
The ethylene propylene diene monomer is K2650C of Allandiaceae;
the carbon black N550/N774 is SPSO/N774 of cabot;
the argil N85 is a Hoffman product N85;
the polyisobutylene is H-100 of INEOS;
the zinc oxide is AZO-805 of Taiwan diligent;
the stearic acid is a product 1801 of Indonesia;
the peroxide vulcanizing agent BIBP is PERKADOX 14S-FL;
the peroxide auxiliary crosslinking agent butadiene rubber BR9000 is a universal grade butadiene rubber on the market.
The preparation method of the environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding can comprise the following steps:
step 1: putting ethylene propylene diene monomer and peroxide co-crosslinking agent butadiene rubber BR9000 into an internal mixer, mixing to 80 ℃, then sequentially putting carbon black N550, carbon black N774, pottery clay N85, polyisobutylene, zinc oxide, stearic acid and an antioxidant SP-P into the internal mixer according to the mixture ratio, mixing for 10-12 minutes, and mixing to about 130 ℃ to obtain uniform master batch;
step 2: standing the master batch for 24 hours, cooling, then putting the master batch into an internal mixer, adding a peroxide vulcanizing agent BIBP, mixing to 85 ℃, discharging, introducing into an open mill, turning and discharging, and cooling by a cooling machine to obtain a final rubber sheet;
and step 3: and (3) cutting the final rubber sheet to the width required by production, inspecting and using the final rubber sheet for automatic machine production after qualification, and performing vulcanization molding to obtain an ideal demolding effect.
And 4, step 4: and after the product is formed, the product is subjected to secondary vulcanization (capable of being baked in an oven) at 150 ℃ for 4 hours, so that small molecules in the product are fully volatilized, and the obtained product can meet the requirements of application occasions related to application water.
Example 2
The difference between the embodiment and the embodiment 1 is that the raw materials are mixed according to the following mixture ratio: 100 parts of ethylene propylene diene monomer, 40 parts of carbon black N550, 50 parts of carbon black N774, 20 parts of argil, 20 parts of polyisobutene, 5 parts of zinc oxide, 1 part of stearic acid, 0.8 part of anti-aging agent SP-P, 3 parts of peroxide BIBP and 900015 parts of butadiene rubber BR.
The product in this example had an ideal demolding effect. The obtained product after the secondary vulcanization can meet the requirements of application occasions related to application water.
Example 3
The difference between the embodiment and the embodiment 1 is that the raw materials are mixed according to the following mixture ratio: 100 parts of ethylene propylene diene monomer, 40 parts of carbon black N550, 77445 parts of carbon black N77445 parts, 25 parts of pottery clay, 20 parts of polyisobutene, 5 parts of zinc oxide, 1 part of stearic acid, 0.8 part of anti-aging agent SP-P, 3 parts of peroxide BIBP and 90002 parts of butadiene rubber BR.
The product in the embodiment has an unsatisfactory demolding effect and a mold sticking phenomenon. The obtained product after the secondary vulcanization can meet the requirements of application occasions related to application water.
Example 4
The difference between the embodiment and the embodiment 1 is that the raw materials are mixed according to the following mixture ratio: 100 parts of ethylene propylene diene monomer, 40 parts of carbon black N550, 77445 parts of carbon black N77425 parts, 8525 parts of pottery clay, 20 parts of polyisobutene, 5 parts of zinc oxide, 1 part of stearic acid, 0.8 part of antioxidant SP-P, 3 parts of peroxide BIBP and 900020 parts of peroxide assistant crosslinking agent BR.
The product in the embodiment has ideal demolding effect, but the hardness of the product is obviously increased and is not easy to control. The obtained product after the secondary vulcanization can meet the requirements of application occasions related to application water.
Four groups of samples were prepared in the above four groups of examples, and the test results are shown in table 1 below.
TABLE 1
The above embodiments are not intended to limit the form and style of the present invention, and any suitable changes or modifications made by those skilled in the art should be considered as not departing from the scope of the present invention.
Claims (9)
1. The environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding is characterized by comprising the following raw materials in parts by weight, based on 100 parts by weight of rubber virgin rubber: 90-105 parts of ethylene propylene diene monomer, 30-40 parts of carbon black N550, 40-50 parts of carbon black N774, 10-20 parts of pottery clay N85, 10-30 parts of polyisobutylene, 2-5 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.6-0.8 part of anti-aging agent SP-P, 1.5-3 parts of peroxide vulcanizing agent BIBP and 5-15 parts of peroxide co-crosslinking agent butadiene rubber BR 9000.
2. The environmentally friendly peroxide vulcanized EPDM material suitable for automatic mold release according to claim 1 wherein:
the ethylene propylene diene monomer is K2650C of Allandiaceae;
the carbon black N550/N774 is SPSO/N774 of Cabot;
the argil N85 is a Hoffman product N85;
the polyisobutylene is H-100 of INEOS;
the zinc oxide is AZO-805 of Taiwan diligent;
the stearic acid is a product 1801 of Indonesia;
the peroxide vulcanizing agent BIBP is PERKADOX 14S-FL;
the peroxide auxiliary crosslinking agent butadiene rubber BR9000 is a universal grade butadiene rubber on the market.
3. The environmentally friendly peroxide vulcanized EPDM material suitable for automatic mold release according to claim 1 wherein: 100 parts of ethylene propylene diene monomer, 35 parts of carbon black N550, 45 parts of carbon black N774, 15 parts of pottery clay N85, 15 parts of polyisobutylene, 3 parts of zinc oxide, 0.5 part of stearic acid, 0.7 part of anti-aging agent SP-P, 2 parts of peroxide vulcanizing agent BIBP and 10 parts of peroxide co-crosslinking agent butadiene rubber BR 9000.
4. The environmentally friendly peroxide vulcanized EPDM material suitable for automatic mold release according to claim 1 wherein: 100 parts of ethylene propylene diene monomer, 40 parts of carbon black N550, 50 parts of carbon black N774, 20 parts of pottery clay N85, 20 parts of polyisobutylene, 5 parts of zinc oxide, 1 part of stearic acid, 0.8 part of an anti-aging agent SP-P, 3 parts of peroxide vulcanizing agent BIBP and 15 parts of peroxide co-crosslinking agent butadiene rubber BR 9000.
5. The preparation method of the environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding is characterized in that the environment-friendly peroxide vulcanized EPDM material suitable for automatic demolding comprises the following raw material components in parts by weight: 90-105 parts of ethylene propylene diene monomer, 30-40 parts of carbon black N550, 40-50 parts of carbon black N774, 10-20 parts of pottery clay N85, 10-30 parts of polyisobutylene, 2-5 parts of zinc oxide, 0.5-2 parts of stearic acid, 0.6-0.8 part of anti-aging agent SP-P, 1.5-3 parts of peroxide vulcanizing agent BIBP and 5-15 parts of peroxide co-crosslinking agent butadiene rubber BR 9000;
the preparation method comprises the following steps:
step 1: firstly, putting ethylene propylene diene monomer and peroxide co-crosslinking agent butadiene rubber BR9000 into an internal mixer, mixing to 80 ℃, then sequentially adding other raw materials except peroxide vulcanizing agent BIBP for mixing, and mixing to about 130 ℃ to obtain uniform master batch;
step 2: after the master batch is kept stand and cooled, adding peroxide vulcanizing agent BIBP according to a proportion, mixing to 85 ℃, discharging, introducing into an open mill, turning over and discharging, and cooling to obtain a final rubber sheet;
and step 3: vulcanizing the final rubber sheet to form a product, and demolding;
and 4, step 4: and the product is subjected to secondary vulcanization at 150 ℃ for 4 hours after being formed.
6. The method for preparing the environmentally friendly peroxide vulcanized EPDM material suitable for automatic demolding according to claim 5, wherein the method comprises the following steps: in the step 1, the rubber mixing temperature is controlled below 130 ℃, and the mixing time is 10-12 minutes.
7. The method for preparing the environmentally friendly peroxide vulcanized EPDM material suitable for automatic mold release according to claim 5, wherein the method comprises the following steps: in the step 2, the master batch and the peroxide vulcanizing agent BIBP are mixed by an open mill or an internal mixer, and the mixing and discharging temperature of the internal mixer is controlled below 85 ℃.
8. The method for preparing the environmentally friendly peroxide vulcanized EPDM material suitable for automatic mold release according to claim 5, wherein the method comprises the following steps: and step 3, injection molding or compression molding the final rubber sheet at 182 +/-5 ℃ to obtain the product.
9. The method of claim 8, wherein the EPDM material is formulated as an environmentally friendly peroxide-vulcanized EPDM material suitable for automated demolding, and further comprises: and 3, cutting the final rubber sheet into corresponding strip-shaped rubber materials according to the required specification of the product, and then forming the strip-shaped rubber materials into the product in a mold at high temperature.
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| CN109096624A (en) * | 2018-08-30 | 2018-12-28 | 青岛三祥科技股份有限公司 | A kind of rubber composition and preparation method thereof for automotive hose rubber core |
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