A solar laminate composite AEM rubber sheet and its preparation process

Abstract

This invention provides a composite AEM rubber sheet for a solar laminate. The rubber sheet comprises, from top to bottom, a non-working surface rubber sheet, a skeleton mesh layer, and a working surface rubber sheet, which are vulcanized together. The non-working surface rubber sheet is an EPDM rubber sheet. The working surface rubber sheet mainly comprises the following components by weight: 100 parts AEM-DP, 50-80 parts carbon black, 1-2 parts antioxidant, 2-5 parts internal release agent, 0.5-1.5 parts anti-scorching agent, 5-7 parts peroxide vulcanizing agent, and 1.5-3 parts crosslinking agent. The preparation process includes the following steps: S1, preparing AEM compound and EPDM compound separately; S2, extruding the working surface semi-finished rubber sheet and the non-working surface semi-finished rubber sheet separately; S3, vulcanizing the working surface semi-finished rubber sheet, the skeleton mesh layer, and the non-working surface semi-finished rubber sheet together to form a composite AEM rubber sheet. This invention's three-layer structure can be vulcanized in one step, simplifying the process, effectively reducing the production cost of AEM rubber sheets, and improving production efficiency.

Description

Technical Field

[0001] This invention relates to the field of rubber sheet preparation technology, and in particular to a solar laminate composite AEM rubber sheet and its preparation process. Background Technology

[0002] AEM rubber, short for ethylene acrylate rubber, is a copolymer of ethylene and methyl acrylate (Methyl acrylate) with a content of 8%–40%. It is a milky white, semi-transparent solid, a synthetic rubber composed of ethylene and acrylic monomers. Ethylene provides good low-temperature performance, while the acrylic portion enhances oil resistance. The combination of the saturated main chain and polar side groups also provides good heat resistance, ozone resistance (weather resistance), and resistance to many chemicals.

[0003] AEM rubber is widely used in automotive rubber parts, including AEM binary and AEM ternary rubbers. Among them, AEM ternary rubber exhibits excellent flexural strength, with a flexural life exceeding 250,000 cycles at 100℃. Its dynamic performance is also good, with high-temperature damping performance approaching that of IIR rubber. AEM rubber also demonstrates excellent resistance to compression set, especially AEM ternary rubber vulcanized with amine-based vulcanizing agents, which exhibits less than 20% compression set at 170℃ for 70 hours. In contrast, binary rubber vulcanized with peroxides shows slightly lower resistance to compression set compared to ternary rubber.

[0004] Our company has optimized the selection of the main rubber, plasticizer, and vulcanization accelerator in the formulation design of AEM ternary rubber. In terms of process, we have improved the two-stage vulcanization and developed an oil-resistant and high-temperature resistant rubber sheet for solar laminators. It can be used as a laminator sheet and has excellent performance at high temperatures of 170 degrees Celsius and above.

[0005] The high price of oil-resistant and high-temperature resistant rubber sheets for solar laminators made from AEM ternary adhesive limits their application range and prevents their widespread use and promotion in the low-to-mid-end laminator market. Therefore, optimizing the oil-resistant and high-temperature resistant rubber sheets through technical means to reduce production costs and expand their application range is the primary goal at this stage. Summary of the Invention

[0006] This invention provides a solar laminate composite AEM rubber sheet and its preparation process, which can meet the heat resistance requirements of the rubber sheet and effectively reduce the production cost of the AEM rubber sheet.

[0007] One technical solution adopted by the present invention is to provide a solar laminate composite AEM rubber sheet, wherein the rubber sheet comprises a non-working surface rubber sheet, a skeleton grid layer and a working surface rubber sheet arranged sequentially from top to bottom, and the three are vulcanized and composited.

[0008] The non-working surface adhesive sheet mainly comprises the following components in parts by weight:

[0009] 100 parts EPDM rubber, 50-65 parts carbon black, 5-8 parts paraffin oil, 20-30 parts inorganic filler, 5-10 parts zinc oxide, 0.5-1.0 parts stearic acid, 4.5-9 parts antioxidant, 2-4 parts tackifying resin, 2-4 parts coupling agent, 8-10 parts peroxide vulcanizing agent, and 3-5 parts co-crosslinking agent;

[0010] The working surface rubber sheet mainly comprises the following components in parts by weight:

[0011] 100 parts AEM-DP, 50-80 parts carbon black, 1-2 parts antioxidant, 2-5 parts internal release agent, 0.5-1.5 parts anti-scorching agent, 5-7 parts peroxide vulcanizing agent, and 1.5-3 parts crosslinking agent.

[0012] Furthermore, the skeleton mesh layer is made of aramid mesh fabric skeleton material.

[0013] Furthermore, the peroxide vulcanizing agent is one of DCP vulcanizing agent, BIPB vulcanizing agent, and 25 vulcanizing agent.

[0014] Furthermore, the peroxide vulcanizing agent is a bis25 vulcanizing agent, which is a vulcanizing agent with a bis25 content of 50%.

[0015] Furthermore, the crosslinking agent is one of TAC crosslinking agent, TAIC crosslinking agent, TMPTMA crosslinking agent, and HVA-2 crosslinking agent.

[0016] Furthermore, the crosslinking agent used is TAIC crosslinking agent, which has the best overall performance when combined with 25 vulcanizing agent.

[0017] Another technical solution adopted by the present invention is: providing a preparation process for a solar laminate composite AEM rubber sheet, comprising the following steps:

[0018] S1. Prepare AEM compound and EPDM compound respectively;

[0019] S2. Extrude or calender AEM compound and EPDM compound respectively to obtain semi-finished rubber sheets for working surface and non-working surface.

[0020] S3. Tension the skeleton mesh layer and cover it on the semi-finished rubber sheet on the working surface, cover the semi-finished rubber sheet on the non-working surface with the skeleton mesh layer, and vulcanize together to obtain a composite AEM rubber sheet.

[0021] Furthermore, in step S1, the preparation of AEM compound includes the following steps:

[0022] SA1, Mixing Masterbatch: AEM-DP, antioxidant, internal release agent, anti-scorching agent and carbon black are put into the internal mixer. The internal mixer is mixed by gradually reducing the speed in stages. The AEM masterbatch is obtained by discharging the rubber.

[0023] SA2, One-time refining: Add AEM masterbatch to the open mill for refining. After refining evenly, sheet out and cool.

[0024] SA3, Vulcanization and Mixing: Add the AEM masterbatch, vulcanizing agent and crosslinking agent after one refining into a two mill or internal mixer for mixing, and discharge the rubber to obtain AEM compound.

[0025] SA4, Secondary Refining: Add the AEM compound to the open mill for refining. After refining evenly, sheet out and cool.

[0026] Furthermore, in the mixing process described in step SA1, the pressure of the top plug is set between 4.5-5.5 KGF, the filling coefficient is between 0.7-0.75, and the step-by-step speed reduction refers to the speed of the internal mixer being gradually reduced from the initial 35 to 25 before discharge, after each top plug is raised for cleaning, and the discharge temperature is controlled between 135-145℃.

[0027] Furthermore, in the mixing process described in step SA3, the pressure of the top plug is set between 3.5-4.5 KGF, the water temperature in the three zones is controlled within 20℃, the rotation speed is between 15-25 R / MIN, the filling coefficient is between 0.5-0.65, and the discharge temperature is controlled within 100℃, and the AEM compound is obtained by discharge.

[0028] The beneficial effects of this invention, which describes a solar laminate composite AEM rubber sheet and its preparation process, are as follows:

[0029] 1. The use of AEM and EPDM composite molding rubber sheet enables the working surface to work well under 170℃×70h conditions, and effectively reduces the production cost of AEM rubber sheet, making it more widely used and promoted in the low-to-mid-end laminator market.

[0030] 2. Due to the good adhesion between the semi-finished rubber sheet on the working surface and the skeleton material, the three-layer structure can be vulcanized and molded in one step during the preparation of this composite AEM rubber sheet, which greatly simplifies the process and improves production efficiency. Attached Figure Description

[0031] Figure 1 This is a preparation process of a solar laminate composite AEM rubber sheet according to the first embodiment of the present invention;

[0032] Figure 2 This is a comparison table of AEM compound performance test data from various embodiments of the present invention. Detailed Implementation

[0033] The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby providing a clearer and more explicit definition of the scope of protection of the present invention.

[0034] The first embodiment of the present invention provides a solar laminate composite AEM rubber sheet, the rubber sheet comprising a non-working surface rubber sheet, a skeleton grid layer and a working surface rubber sheet arranged sequentially from top to bottom, the three being vulcanized and composited;

[0035] The non-working surface adhesive sheet mainly comprises the following components by weight:

[0036] 100 parts EPDM rubber, 57 parts carbon black, 6 parts paraffin oil, 25 parts inorganic filler, 7 parts zinc oxide, 0.7 parts stearic acid, 6 parts antioxidant, 3 parts tackifying resin, 3 parts coupling agent, 9 parts peroxide vulcanizing agent, and 4 parts co-crosslinking agent.

[0037] The carbon black comprises 45 parts N330 and 12 parts silica 255, the paraffin oil is high flash point paraffin oil P2280, the inorganic filler is calcined kaolin, the antioxidant is a combination of RD, MBI and 445 (1:1:1), the tackifying resin is C5, the coupling agent is SI69-50, the peroxide curing agent is bis-25 curing agent (101-50 powder containing 50% bis-25), and the crosslinking agent is TMPTMA crosslinking agent (350D TMPTMA-50).

[0038] The working surface rubber sheet mainly comprises the following components by weight:

[0039] 100 parts AEM binary rubber, 65 parts carbon black, 1.5 parts antioxidant, 3 parts internal release agent, 1 part anti-scorching agent, 6 parts peroxide vulcanizing agent, and 2 parts crosslinking agent;

[0040] The main adhesive is AEM-DP, the carbon black consists of 45 parts N550 and 20 parts N774, the antioxidant is 445, the internal release agent is a mixture of stearic acid, VAM and PE wax (1:3:2), the anti-scorching agent is 18D, the peroxide curing agent is bis25 curing agent (101-50 powder containing 50% bis25), and the crosslinking agent is TAIC crosslinking agent (TAIC-70).

[0041] The skeleton mesh layer uses aramid mesh fabric as the skeleton material. This aramid mesh fabric skeleton material is pre-treated and impregnated with rubber, which can bond well with AEM and EPDM compound rubber, thereby improving the flexural fatigue and service life of the rubber sheet.

[0042] In the research on AEM and EPDM composites, based on the characteristic that both AEM binary rubber and EPDM rubber compounds can be vulcanized using peroxides, AEM binary rubber was selected as the main rubber compound for the working surface rubber sheet. This provides a theoretical basis for the simultaneous vulcanization of the working surface rubber sheet and the non-working surface rubber sheet. Based on this, experiments and analyses were conducted on the specific binary rubber type used in the AEM compound.

[0043] Among AEM binary adhesives, Vamac DP has performance closer to that of AEM ternary adhesives, also possessing good oil and high temperature resistance, good compression set resistance, and good low temperature elasticity. However, Vamac DHC has insufficient heat resistance (the upper limit of continuous working temperature for ordinary Vamac elastomers is 165℃). Therefore, to ensure good operation under conditions of 170℃×70h, AEM-DP should be selected as the main adhesive for the working surface.

[0044] Peroxide vulcanizing agents suitable for AEM-DP binary rubber include DCP vulcanizing agent, BIPB vulcanizing agent (BIPB is odorless DCP, 1,3-di-tert-butylperoxydiisopropylbenzene), and bis25 vulcanizing agent (bis25 is DBPMH, 2,5-dimethyl-2,5-di-tert-butylperoxyhexane):

[0045] The 10-hour half-life temperatures of these three most commonly used industrial peroxides are DCP: 117℃, BIPB: 120℃, and DBPMH: 122℃. These temperatures are the safe operating temperatures of the rubber compound. The higher the temperature, the better the operating safety. In this embodiment, both the working surface rubber sheet and the non-working surface rubber sheet use 25 as the peroxide vulcanizing agent, which provides better operating safety.

[0046] Among them, the 25 vulcanizing agent is a vulcanizing agent with a 25 content of 50%, which is formed by the adsorption of liquid 25 by inorganic matter.

[0047] Commonly used crosslinking agents for peroxides include TAC (tartrate cyanurate), TAIC (tartrate isocyanurate), TMPTMA (trimethylolpropane trimethacrylate), and HVA-2 (N,N-m-phenylene bismaleimide).

[0048] Four types of crosslinking agents were tested in combination with 25 vulcanizing agent. Each of them had its own advantages in terms of scorch safety, heat resistance, physical and mechanical properties, resilience and compression set, and flexural fatigue resistance. In this embodiment, TAIC crosslinking agent was selected as the crosslinking agent. The rubber compound prepared by combining it with 25 vulcanizing agent had the best overall performance.

[0049] Please see Figure 1 The first embodiment of the present invention provides a process for preparing a solar laminate composite AEM rubber sheet, comprising the following steps:

[0050] S1. Prepare AEM compound and EPDM compound respectively;

[0051] S2. Extrude AEM compound and EPDM compound separately to obtain semi-finished rubber sheets for the working surface and non-working surface.

[0052] S3. Lay several semi-finished rubber sheets on the working surface overlapping on the flat vulcanizing machine, tension the skeleton grid layer and cover it, then lay the semi-finished rubber sheets on the non-working surface overlapping on the skeleton grid layer, and vulcanize them together to obtain composite AEM rubber sheets.

[0053] In step S1, the preparation of AEM compound includes the following steps:

[0054] SA1, Mixing Masterbatch: AEM-DP, antioxidant 445, internal release agent (stearic acid, VAM, PE wax), anti-scorching agent 18D and carbon black (N550, N774) are put into the internal mixer. The top jack pressure is set to 5KGF and the filling coefficient is 0.7. The internal mixer is mixed by gradually reducing the speed in stages, from the initial 35 to 25 before discharge. The top jack is raised and cleaned each time, and then gradually reduced. The discharge temperature is controlled at 140℃. The AEM masterbatch is obtained by discharge.

[0055] SA2, One-time refining: Add AEM masterbatch to the open mill for refining. After refining evenly, sheet out and cool, and let stand for more than 8 hours.

[0056] SA3, Vulcanization and Mixing: Add the AEM masterbatch after one round of mixing, double 25 vulcanizing agent and TAIC crosslinking agent into the internal mixer for mixing. Set the top jack pressure to 4KGF, control the water temperature in the three zones to below 20℃, the rotation speed to 20R / MIN, the filling factor to 0.55, and discharge the rubber below 95℃ to obtain the AEM compound.

[0057] SA4, Secondary Refining: Add the AEM compound to the open mill for refining. After refining evenly, sheet out and cool. Let it stand for more than 24 hours to eliminate the sheeting stress of the rubber compound, and to fully impregnate, disperse and shrink, ensuring the dimensional stability of the semi-finished product.

[0058] AEM compound performance test data in this embodiment:

[0059]

[0060]

[0061] *Refers to the AEM compound after one stage of vulcanization. The vulcanization process is: 180℃ × 8 minutes. Performance test data for the EPDM compound in this embodiment:

[0062]

[0063] *Refers to the first stage of vulcanized EPDM compound. First stage vulcanization process: 180℃×8MIN.

[0064] The composite AEM rubber sheet prepared in this embodiment has a service life of over 150,000 cycles.

[0065] In the second to sixth embodiments of the present invention, the selection of peroxide vulcanizing agent and crosslinking agent in AEM compound was adjusted, and the mass ratios of each embodiment are shown in the following figure:

[0066]

[0067] Using the same preparation process as in the first embodiment, the performance test data of the AEM compound for each embodiment are shown in the table below:

[0068]

[0069]

[0070] The comparison of the various embodiments shows that the overall performance is best when the peroxide vulcanizing agent and the crosslinking agent are selected to be used in combination with 25 and TAIC.

[0071] The beneficial effects of this invention, which describes a solar laminate composite AEM rubber sheet and its preparation process, are as follows:

[0072] 1. The use of AEM and EPDM composite molding rubber sheet enables the working surface to work well under 170℃×70h conditions, and effectively reduces the production cost of AEM rubber sheet, making it more widely used and promoted in the low-to-mid-end laminator market.

[0073] 2. Due to the good adhesion between the semi-finished rubber sheet on the working surface and the skeleton material, the three-layer structure can be vulcanized and molded in one step during the preparation of this composite AEM rubber sheet, which greatly simplifies the process and improves production efficiency.

[0074] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural or procedural transformations made based on the content of the present invention's specification and drawings, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. A solar laminate composite AEM rubber sheet, the rubber sheet comprising a non-working surface rubber sheet, a skeleton grid layer and a working surface rubber sheet arranged sequentially from top to bottom, the three being vulcanized and composited; The non-working surface adhesive sheet mainly comprises the following components in parts by weight: 100 parts EPDM rubber, 50-65 parts carbon black, 5-8 parts paraffin oil, 20-30 parts calcined kaolin, 5-10 parts zinc oxide, 0.5-1.0 parts stearic acid, 4.5-9 parts antioxidant, 2-4 parts tackifying resin, 2-4 parts coupling agent, 8-10 parts peroxide vulcanizing agent, and 3-5 parts co-crosslinking agent; The working surface rubber sheet mainly comprises the following components in parts by weight: 100 parts AEM-DP, 50-80 parts carbon black, 1-2 parts antioxidant, 2-5 parts internal release agent, 0.5-1.5 parts anti-scorching agent, 5-7 parts peroxide vulcanizing agent, and 1.5-3 parts crosslinking agent.

2. The solar laminate composite AEM rubber sheet according to claim 1, characterized in that, The skeleton mesh layer uses aramid mesh fabric as the skeleton material.

3. A solar laminate composite AEM rubber sheet according to claim 1 or 2, characterized in that, The peroxide vulcanizing agent is one of DCP vulcanizing agent, BIPB vulcanizing agent, and 25-25 vulcanizing agent.

4. The solar laminate composite AEM rubber sheet according to claim 3, characterized in that, The peroxide vulcanizing agent used is a double 25 vulcanizing agent.

5. The solar laminate composite AEM rubber sheet according to claim 4, characterized in that, The crosslinking agent is one of TAC crosslinking agent, TAIC crosslinking agent, TMPTMA crosslinking agent, and HVA-2 crosslinking agent.

6. The solar laminate composite AEM rubber sheet according to claim 5, characterized in that, The crosslinking agent used is TAIC crosslinking agent.

7. A process for preparing the solar laminate composite AEM rubber sheet according to claim 1, comprising the following steps: S1. Prepare AEM compound and EPDM compound respectively; S2. Extrude or calender AEM compound and EPDM compound respectively to obtain semi-finished rubber sheets for working surface and non-working surface. S3. Tension the skeleton mesh layer and cover it on the semi-finished rubber sheet on the working surface, cover the semi-finished rubber sheet on the non-working surface with the skeleton mesh layer, and vulcanize together to obtain a composite AEM rubber sheet.

8. The preparation process of a solar laminate composite AEM rubber sheet according to claim 7, characterized in that, In step S1, the preparation of AEM compound includes the following steps: SA1, Mixing Masterbatch: AEM-DP, antioxidant, internal release agent, anti-scorching agent and carbon black are put into an internal mixer. The internal mixer is mixed by gradually reducing the speed in stages. The AEM masterbatch is obtained by discharging the rubber. SA2, One-time refining: Add AEM masterbatch to the open mill for refining. After refining evenly, sheet out and cool. SA3, Vulcanization and Mixing: Add the AEM masterbatch, vulcanizing agent and crosslinking agent after one refining into a two mill or internal mixer for mixing, and discharge the rubber to obtain AEM compound. SA4, Secondary Refining: Add the AEM compound to the open mill for refining. After refining evenly, sheet out and cool.

9. The preparation process of a solar laminate composite AEM rubber sheet according to claim 8, characterized in that, In the mixing process described in step SA1, the pressure of the top plug is set between 4.5-5.5 kgf, the filling coefficient is between 0.7-0.75, and the discharge temperature is controlled between 135-145℃.

10. The preparation process of a solar laminate composite AEM rubber sheet according to claim 8, characterized in that, In the mixing process described in step SA3, the pressure of the top plug is set between 3.5-4.5 kgf, the water temperature in the three zones is controlled within 20℃, the rotation speed is between 15-25 r / min, the filling coefficient is between 0.5-0.65, and the discharge temperature is controlled within 100℃, and the AEM compound is obtained by discharge.

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