CN115975302A - Chlorinated polyethylene rubber composition, rubber sheet and preparation method - Google Patents
Chlorinated polyethylene rubber composition, rubber sheet and preparation method Download PDFInfo
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- 229920006235 chlorinated polyethylene elastomer Polymers 0.000 title claims abstract description 97
- 229920001971 elastomer Polymers 0.000 title claims abstract description 67
- 239000000203 mixture Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 40
- 238000004073 vulcanization Methods 0.000 claims abstract description 32
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 24
- 239000004014 plasticizer Substances 0.000 claims abstract description 18
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 16
- 239000011256 inorganic filler Substances 0.000 claims abstract description 16
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 16
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 16
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 10
- 239000000194 fatty acid Substances 0.000 claims abstract description 10
- 229930195729 fatty acid Natural products 0.000 claims abstract description 10
- -1 compound fatty acid Chemical class 0.000 claims abstract description 5
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 4
- 150000001875 compounds Chemical class 0.000 claims abstract 2
- 238000002156 mixing Methods 0.000 claims description 67
- 238000003490 calendering Methods 0.000 claims description 59
- 239000000047 product Substances 0.000 claims description 33
- 238000007599 discharging Methods 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 239000006229 carbon black Substances 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 16
- 239000004709 Chlorinated polyethylene Substances 0.000 claims description 15
- 238000013329 compounding Methods 0.000 claims description 15
- 238000005096 rolling process Methods 0.000 claims description 14
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 8
- 239000008116 calcium stearate Substances 0.000 claims description 8
- 235000013539 calcium stearate Nutrition 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000011265 semifinished product Substances 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 7
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 7
- 238000010030 laminating Methods 0.000 claims description 7
- DCIYMHRRSZGEQI-UHFFFAOYSA-N B([O-])([O-])[O-].[Zn+2].O.O.O.O.O.O.O.O.O.O.B([O-])([O-])[O-].[Zn+2].[Zn+2] Chemical compound B([O-])([O-])[O-].[Zn+2].O.O.O.O.O.O.O.O.O.O.B([O-])([O-])[O-].[Zn+2].[Zn+2] DCIYMHRRSZGEQI-UHFFFAOYSA-N 0.000 claims description 6
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 6
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 6
- JNXDCMUUZNIWPQ-UHFFFAOYSA-N trioctyl benzene-1,2,4-tricarboxylate Chemical compound CCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC)C(C(=O)OCCCCCCCC)=C1 JNXDCMUUZNIWPQ-UHFFFAOYSA-N 0.000 claims description 5
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 150000004867 thiadiazoles Chemical class 0.000 claims description 4
- IPJGAEWUPXWFPL-UHFFFAOYSA-N 1-[3-(2,5-dioxopyrrol-1-yl)phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC(N2C(C=CC2=O)=O)=C1 IPJGAEWUPXWFPL-UHFFFAOYSA-N 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims 2
- 239000003973 paint Substances 0.000 claims 2
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- 229910052759 nickel Inorganic materials 0.000 claims 1
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- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 7
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000004610 Internal Lubricant Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- BQHTWZRFOSRCCH-UHFFFAOYSA-L nickel(2+);dicarbamodithioate Chemical compound [Ni+2].NC([S-])=S.NC([S-])=S BQHTWZRFOSRCCH-UHFFFAOYSA-L 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of vulcanized rubber, and particularly discloses a chlorinated polyethylene rubber composition, a rubber plate and a preparation method. The chlorinated polyethylene rubber composition comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber, 2-15 parts of heat stabilizer, 0.1-0.5 part of anti-aging agent, 10-60 parts of reinforcing agent, 20-80 parts of inorganic filler, 2-6 parts of flow promoter, 10-35 parts of plasticizer, 2-5 parts of cross-linking agent and 1-5 parts of auxiliary cross-linking agent; the flow auxiliary agent is compound fatty acid R-300V. The flow assistant R-300V has obvious internal lubrication effect on a rubber compound system, the demolding performance and the mechanical property of the plate in a rubber plate vulcanization process are greatly improved, the rubber plate with a smooth and flat surface and extremely small shrinkage deformation can be prepared by a drum type vulcanizing machine and a flat plate vulcanizing machine, and a finished product of the rubber plate has good mechanical property, heat resistance, aging resistance, flame retardance and oil resistance, is a multifunctional low-cost rubber plate, and expands the application field of the chlorinated polyethylene rubber.
Description
Technical Field
The invention relates to the technical field of vulcanized rubber, in particular to a chlorinated polyethylene rubber composition, a rubber plate and a preparation method thereof.
Background
The rubber sheet is a sheet product with a certain thickness and a large area, which is prepared by using rubber as a main material (which can contain reinforcing materials such as fabric, metal mesh and the like) through calendering, laminating, molding or extrusion molding and vulcanizing by a flat plate vulcanizing machine or a drum vulcanizing machine continuously, and is used for laying sealing gaskets, damping and noise reduction sheets, rubber bag bags, workbenches and floors. The requirements for the rubber sheet material are also different according to different use conditions. Some working conditions require that the rubber sheet has special properties such as flame retardance, oil resistance, resistance to various chemical media, ozone resistance, weather resistance, high temperature resistance, low temperature resistance and the like besides certain physical and mechanical properties, and sometimes the rubber sheet needs to have several special properties to meet the use requirements.
Chlorinated polyethylene rubber (CPE) is a saturated polymeric material. Chlorinated polyethylene rubber products in the current market are of thermoplastic type and vulcanization type, wherein the thermoplastic type chlorinated polyethylene rubber has poor heat resistance and large deformability; the vulcanized chlorinated polyethylene rubber is prepared by vulcanizing rubber materials, and has good performances of heat aging resistance, ozone resistance, weather resistance, oil resistance, chemical medium resistance, flame retardance and the like. However, the method has the defects of uneven surface, large shrinkage, mold adhesion and the like during mold vulcanization, and is only used for non-model products such as wires, cables, rubber tubes and the like at present, so that the chlorinated polyethylene rubber plate cannot be continuously produced on a flat vulcanizing machine and a drum vulcanizing machine.
Disclosure of Invention
Aiming at the problems of the existing chlorinated polyethylene rubber, the invention provides a chlorinated polyethylene rubber composition, a vulcanized chlorinated polyethylene rubber sheet and a preparation method, wherein the chlorinated polyethylene rubber is prepared by adding compounding agents into the chlorinated polyethylene rubber: the composite fatty acid R-300V flow assistant, the heat stabilizer, the anti-aging agent, the reinforcing agent, the inorganic filler, the plasticizer, the crosslinking agent and the auxiliary crosslinking agent are cooperated, and the prepared vulcanized chlorinated polyethylene rubber plate not only has good performances of heat aging resistance, ozone resistance, weather resistance, oil resistance, various chemical corrosion resistance, flame retardance and the like, but also has smooth and flat surface of the finished plate, excellent physical and mechanical properties, and the cost is obviously lower than that of other products with similar performances, and can replace special rubber plates with high price, thereby being a multifunctional low-cost rubber plate.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
in a first aspect, the invention provides a chlorinated polyethylene rubber composition, which comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber, 2-15 parts of heat stabilizer, 0.1-0.5 part of anti-aging agent, 10-60 parts of reinforcing agent, 20-80 parts of inorganic filler, 2-6 parts of flow promoter, 10-35 parts of plasticizer, 2-5 parts of crosslinking agent and 1-5 parts of auxiliary crosslinking agent;
the flow assistant is compound fatty acid R-300V.
Compared with the prior art, the chlorinated polyethylene rubber composition provided by the invention at least has the following beneficial effects:
(1) According to the chlorinated polyethylene rubber composition provided by the invention, the composite fatty acid R-300V is selected as the flow assistant, so that the demolding property and the mechanical property of the plate in the rubber plate vulcanization process are greatly improved. On one hand, the composite fatty acid R-300V is used as an internal lubricant, so that the calendered film has higher fluidity when the rubber plate is vulcanized, and the vulcanized plate product forms a smooth and flat surface; on the other hand, the compound fatty acid R-300V can form an isolating layer between the calendered film and the vulcanizing machine, so that the calendered film is prevented from deforming due to local die sticking and cannot be made into a flat plate.
(2) According to the chlorinated polyethylene rubber composition provided by the invention, the chlorinated polyethylene rubber is added with the composite fatty acid flow auxiliary agent, the heat stabilizer, the anti-aging agent, the reinforcing agent, the inorganic filler, the plasticizer, the cross-linking agent and the auxiliary cross-linking agent, through specific components and proportion, the components have synergistic effect, the prepared finished plate has a smooth and flat surface and excellent physical and mechanical properties, and has better performances of heat aging resistance, ozone resistance, weather resistance, oil resistance, various chemical corrosion resistance, flame retardance and the like, the product cost is obviously lower than that of other products with similar performances, and the multifunctional low-cost rubber plate can be prepared, and has very important significance for expanding the application field of the chlorinated polyethylene rubber.
Preferably, the chlorinated polyethylene rubber composition comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber, 4-13 parts of heat stabilizer, 0.2-0.4 part of anti-aging agent, 15-55 parts of reinforcing agent, 20-50 parts of inorganic filler, 2-4 parts of flow promoter, 10-25 parts of plasticizer, 2-4 parts of crosslinking agent and 1-3 parts of auxiliary crosslinking agent.
The rubber sheet prepared by adopting the chlorinated polyethylene rubber composition with the optimized formula proportion has higher product flatness, excellent appearance and more excellent performance,
in one embodiment, the chlorinated polyethylene rubber is CPE135B.
In one embodiment, the heat stabilizer is at least one selected from calcium stearate, barium stearate and magnesium oxide.
In one embodiment, the anti-aging agent is N, N' -dibutyl nickel dithiocarbamate (NBC).
In one embodiment, the reinforcing agent is at least one of carbon black N660, carbon black N774, carbon black N990 and white carbon black.
In one embodiment, the inorganic filler is at least one of light calcium carbonate, heavy calcium carbonate, barium sulfate and zinc borate decahydrate.
In one embodiment, the plasticizer is at least one selected from dioctyl phthalate (DOP), tricresyl phosphate (TCP), trioctyl trimellitate (TOTM), and chlorinated paraffin.
In one embodiment, the cross-linking agent is one of bis (1-methyl-1-phenylethyl) peroxide, 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane and thiadiazole derivative ECHO.A.
In one embodiment, the auxiliary crosslinking agent is selected from one of N, N' -m-phenylene maleimide (PDM) and an accelerator 808.
In the present invention, the heat stabilizer, the anti-aging agent, the reinforcing agent, the inorganic filler, the plasticizer, the crosslinking agent and the co-crosslinking agent may be used as conventional compounding agents in the art, but the compounding ratio is within the range defined in the present invention. The preferable types of the compounding agents in the above embodiments can improve the performances of the vulcanized chlorinated polyethylene rubber sheet, such as thermal aging resistance, ozone resistance, weather resistance, oil resistance, various chemical corrosion resistance, flame retardance and the like. The finished product has smooth and flat surface and higher qualification rate.
In a second aspect, the present invention also provides a vulcanized chlorinated polyethylene rubber sheet prepared from the above chlorinated polyethylene rubber composition, based on a general inventive concept.
The vulcanized chlorinated polyethylene rubber plate prepared by the chlorinated polyethylene rubber composition has excellent performances through tests, and the specific parameters are as follows:
the vulcanization characteristics at 165 ℃ for 15min are as follows: t is 10 40-130 seconds, T 90 260-1200 seconds;
the normal temperature physical properties are as follows: the hardness is 60 Shore degree to 85 Shore degree, the tensile strength is 13.5MPa to 18.4MPa, and the elongation at break is 225 percent to 500 percent;
the flame retardant property is as follows: the oxygen index is 30-35;
thermal aging resistance (125 ℃ X96 hours after aging rate of performance): hardness + 3- +9, tensile strength-1.4% - +8.5%, elongation at break-10.6% - + 29.5%;
ozone aging resistance (ozone concentration 100pphm,40 ℃ C.. Times.96 hours, tensile 20%): the surface has no crack;
engine oil resistance (performance change rate after aging at 125 ℃ for 96 hours): the hardness is-6.3 to-2.6, the tensile strength is-11.4 to-1.5 percent, the elongation at break is-14.3 to-21.8 percent, and the mass change rate is +2.0 to +4.4 percent.
In a third aspect, the invention further provides a preparation method of the vulcanized chlorinated polyethylene rubber sheet, which comprises the following preparation steps:
(1) Plasticizing: plasticizing the chlorinated polyethylene rubber by adopting a thin pass method to obtain a chlorinated polyethylene plasticized rubber;
(2) First-stage mixing: adding the chlorinated polyethylene plasticizing rubber, the heat stabilizer, the anti-aging agent, the flow promoter, the reinforcing agent, the inorganic filler and the plasticizer into an internal mixer to perform primary mixing for 6-10 min at the mixing temperature of 110-120 ℃, discharging, uniformly smashing in an open mill, then discharging, and standing to obtain a primary mixing rubber sheet;
(3) And (3) second-stage mixing: carrying out two-stage mixing on the first-stage mixing rubber sheet, the cross-linking agent and the auxiliary cross-linking agent in an internal mixer for 90-120 s, discharging, then uniformly smashing and mixing in an open mill, and then rolling to obtain a two-stage mixing film;
(4) Rolling out a sheet: putting the two-stage mixed roll film into a calender for calendering and sheet discharging, cooling and then coiling to obtain a calendered film;
(5) Vulcanizing the rubber plate: vulcanizing, cooling and coiling the calendered film on a drum vulcanizer by adopting a multilayer film laminating process; or vulcanizing by a flat vulcanizing machine, cooling and cutting edges to obtain the vulcanized chlorinated polyethylene rubber sheet.
The preparation method of the vulcanized chlorinated polyethylene rubber plate provided by the invention adopts the two-stage mixing process by taking the chlorinated polyethylene rubber as a main material and selecting the compound fatty acid as a flow assistant, so that the chlorinated polyethylene rubber material and various compounding agents are more fully mixed, the uniformly dispersed mixed rubber can be obtained, and the finished plate with a smooth and flat surface and excellent physical and mechanical properties can be obtained. Solves the problem that the continuous production on a flat vulcanizing machine and a drum vulcanizing machine can not be realized due to the defects of uneven surface, large contractibility, mold sticking and the like when the chlorinated polyethylene rubber is vulcanized. And the preparation process is simple, easy to control and suitable for large-scale production.
In one embodiment, when the calendered films are vulcanized by a drum vulcanizer in the step (5), the multiple calendered films are separated by guide rollers before entering a main drum, the sum of the thicknesses of the multiple calendered films is 103-105% of the thickness of the finished product, the temperature of the main drum of the drum vulcanizer is 165-170 ℃, steel belt auxiliary heating is adopted, the temperature of the steel belt auxiliary heating is 180-190 ℃, and the finished product is the vulcanized chlorinated polyethylene rubber sheet finally obtained in the step (5).
When a drum vulcanizing machine is adopted for vulcanization, before the rubber sheets enter a main drum, the calendering rubber sheets are soft in material, the calendering rubber sheets are easy to adhere, air bubbles can be generated, and the appearance and the performance of a vulcanized product are influenced. Therefore, before entering the main drum, the multi-layer calendered films are separated by the guide roller, so that the adhesion of the calendered films and the generation of bubbles can be effectively prevented, and the preparation of high-quality plate products with smooth appearance and no bubbles is facilitated. In addition, the tension of each laminated film before entering the main drum needs to be kept consistent, so that the thickness, the flatness and the stretching state of each laminated film are basically the same, and the preparation of a plate product with excellent appearance is facilitated.
When a drum vulcanizer is adopted for vulcanization, the vulcanization time is controlled by the rotating speed of the main drum, and the higher the rotating speed of the main drum is, the smaller the vulcanization time is. The rotational speed of the primary drum is determined from the primary drum diameter, primary drum wrap angle and measured process positive cure time.
In one embodiment, when the calendered film is vulcanized by a flat vulcanizing machine in the step (5), a multi-layer calendered film is pre-compounded by a film compounding machine into a semi-finished product with the thickness of 110% -120% of the finished product and the width of 90% -95% of the finished product, the weight of a single semi-finished product is 102% -107% of the weight of the finished product, the vulcanization temperature is 165% -170 ℃, the pan mouth temperature of the flat vulcanizing machine is less than or equal to 95 ℃, the vulcanization pressure is 2.5-4.0 MPa, and the vulcanization time is 8-15 min, wherein the finished product is the vulcanized chlorinated polyethylene rubber sheet finally obtained in the step (5).
In one embodiment, the plasticizing time in the step (1) is 3 to 5.
The chlorinated polyethylene rubber is in powder form, the powdered chlorinated polyethylene rubber needs to be plasticized at high temperature (within 100 ℃) before formula mixing is carried out, and the plasticized chlorinated polyethylene rubber is in a sheet form, so that the contact area with various compounding agents can be increased, and the full mixing is facilitated.
In one embodiment, the parking time in step (2) is at least 8h.
The standing time after the first mixing is not particularly limited as long as the first mixing piece is cooled to room temperature, generally at least 8h, for example, 8h or 9h 8230, and the like.
In one embodiment, the temperature for the roll-off in step (3) is 55-65 ℃.
In one embodiment, the calendering temperature in the step (4) is 50-60 ℃, and when the drum vulcanizer is used for vulcanization, the thickness of the calendered film is 1-2.5 mm; when the flat vulcanizing machine is used for vulcanizing, the thickness of the calendered film is 2.0 mm-3.5 mm.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the feature. In the description of the invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise. In the description of the present invention, "a plurality" means at least one, e.g., one, two, etc., unless specifically limited otherwise.
The words "preferably," "more preferably," and the like, in the present disclosure mean embodiments of the disclosure that may, in some instances, provide certain benefits. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The following are specific examples, and the starting materials used in the examples are all commercially available products unless otherwise specified. The flow auxiliary agent is R-300V produced by Japan king flower chemical production.
The embodiment of the invention provides a chlorinated polyethylene rubber composition which comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber, 2-15 parts of heat stabilizer, 0.1-0.5 part of anti-aging agent, 10-60 parts of reinforcing agent, 20-80 parts of inorganic filler, 2-6 parts of flow promoter R-300V, 10-35 parts of plasticizer, 2-5 parts of crosslinking agent and 1-5 parts of auxiliary crosslinking agent.
In the embodiment, the heat stabilizer, the anti-aging agent, the reinforcing agent, the inorganic filler, the plasticizer, the crosslinking agent and the auxiliary crosslinking agent can be conventional compounding agents in the field, and the proportion of the compounding agents is within the range.
The preparation method of the chlorinated polyethylene rubber composition for the vulcanized chlorinated polyethylene rubber plate comprises the following preparation steps:
(1) Plasticizing: plasticizing chlorinated polyethylene rubber in an open mill for 3-5 times by adopting a thin pass method, and coating a roll to obtain chlorinated polyethylene plasticized rubber;
(2) First-stage mixing: adding chlorinated polyethylene plasticizing rubber, a heat stabilizer, an anti-aging agent, a flow assistant, a reinforcing agent, an inorganic filler and a plasticizer into an internal mixer to carry out first-stage mixing for 6-10 min at the mixing temperature of 110-120 ℃, discharging, then uniformly mixing in an open mill, then discharging, and standing for at least 8h to obtain a first-stage mixed rubber sheet;
(3) And (3) second-stage mixing: putting the parked first-section mixing rubber sheet into an internal mixer, adding a cross-linking agent and an auxiliary cross-linking agent, mixing for 90-120 s, discharging, uniformly stirring in an open mill, and then rolling at the temperature of 55-65 ℃ to obtain a second-section mixing rubber roll;
(4) Rolling out a sheet: putting the two-stage mixed film into a calender for calendering and sheet discharging, wherein the calendering temperature is 50-60 ℃, the thickness of the calendered film is 1-2.5 mm (vulcanization in a drum vulcanizer), and the thickness of the calendered film is 2.0-3.5 mm (vulcanization in a flat-plate vulcanizer) and is coiled after cooling to obtain the calendered film;
(5) Vulcanizing the rubber plate: vulcanizing by a drum vulcanizing machine: adopting a multi-layer film laminating process, separating the calendered films by adopting a guide roller before the calendered films enter a main drum to prevent adhesion and air inclusion, independently controlling the tension of each layer of calendered film, keeping the tension of the multi-layer calendered films consistent, wherein the sum of the thicknesses of the multi-layer calendered films is 103-105% of the thickness of a finished product, the temperature of the main drum is 165-170 ℃, the auxiliary heating temperature of a steel belt is 180-190 ℃, the speed of a vehicle is converted according to positive vulcanization time and drum diameter, and cooling and coiling are carried out after vulcanization to obtain the product;
vulcanizing by a flat vulcanizing machine: the multi-layer rolled films are pre-compounded into a semi-finished product with the thickness of 110-120% and the width of 90-95% of the finished product by a film compounding machine, the weight of a single semi-finished product is 102-107% of the weight of the finished product, the vulcanization temperature is 165-170 ℃, the vulcanization time is 8-15 min, the pot mouth temperature of a flat vulcanizing machine is less than or equal to 95 ℃, and the vulcanization pressure is 2.5-4.0 MPa.
Example 1
A chlorinated polyethylene rubber composition comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber CPE135B,5 parts of calcium stearate, 10 parts of magnesium oxide, 0.1 part of anti-aging agent NBC,60 parts of carbon black N660, 20 parts of light calcium carbonate, 6 parts of R-300V,10 parts of plasticizer DOP,3 parts of crosslinking agent 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane and 5 parts of co-crosslinking agent PDM.
The preparation method of the chlorinated polyethylene rubber composition for the vulcanized chlorinated polyethylene rubber sheet comprises the following preparation steps:
(1) Plasticizing: plasticizing chlorinated polyethylene rubber in an open mill for 3 times by adopting a thin pass method, and wrapping the chlorinated polyethylene rubber by a roller to obtain chlorinated polyethylene plasticized rubber;
(2) First-stage mixing: adding chlorinated polyethylene plasticizing gum, calcium stearate, magnesium oxide, an anti-aging agent NBC and R-300V into an internal mixer, mixing for 30 seconds, adding carbon black N660, light calcium carbonate and a plasticizer DOP, mixing for 450 seconds at the mixing temperature of 120 ℃, discharging, uniformly stirring in an open mill, discharging, standing for more than 8 hours, and obtaining a section of mixing rubber sheet;
(3) And (3) second-stage mixing: putting the parked first-section mixing rubber sheet into an internal mixer, adding 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and an auxiliary crosslinking agent PDM, mixing for 90 seconds, discharging, uniformly stirring in an open mill, and then rolling at the temperature of 55 ℃ to obtain a second-section mixing rubber film;
(4) Rolling out a sheet: putting the two-stage mixing film into a calender for calendering and sheet discharging, wherein the calendering temperature is 50 ℃, the thickness of the calendered film is 1mm, and cooling and coiling the calendered film to obtain the calendered film;
(5) Vulcanizing the rubber plate: vulcanizing by a drum vulcanizer: the method adopts a multi-layer film laminating process, the rolled films are separated by a guide roller before entering a main drum to prevent adhesion and air inclusion, the tension of each layer of the rolled films is independently controlled, the tension of the multi-layer rolled films is kept consistent, the temperature of the main drum is 165 ℃, the auxiliary heating temperature of a steel belt is 180 ℃, and the multi-layer rolled film is obtained by cooling and coiling after vulcanization.
Example 2
A chlorinated polyethylene rubber composition comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber CPE135B,1 part of calcium stearate, 1 part of barium stearate, 0.3 part of an anti-aging agent NBC,10 parts of carbon black N774, 25 parts of barium sulfate, 20 parts of zinc borate decahydrate, 3.5 parts of a flow aid R-300V,15 parts of tricresyl phosphate (TCP), 8 parts of chlorinated paraffin-40, 5 parts of bis (1-methyl-1-phenylethyl) peroxide and 2 parts of an auxiliary crosslinking agent PDM.
The preparation method of the chlorinated polyethylene rubber composition for the vulcanized chlorinated polyethylene rubber plate comprises the following preparation steps:
(1) Plasticizing: plasticizing chlorinated polyethylene rubber in an open mill for 4 times by adopting a thin pass method, and coating rollers for discharging sheets to obtain chlorinated polyethylene plasticized rubber;
(2) First-stage mixing: adding chlorinated polyethylene plasticizing gum, calcium stearate, barium stearate, an anti-aging agent NBC, barium sulfate and R-300V into an internal mixer, mixing for 60 seconds, adding carbon black N774, zinc borate decahydrate, tricresyl phosphate and chlorinated paraffin-40, mixing for 540 seconds at the mixing temperature of 120 ℃, discharging, then uniformly mixing in an open mill, then discharging, standing for more than 8 hours to obtain a section of mixed rubber sheet;
(3) And (3) second-stage mixing: putting the parked first-section mixing film into an internal mixer, adding a cross-linking agent bis (1-methyl-1-phenethyl) peroxide and an auxiliary cross-linking agent PDM, mixing for 105 seconds, discharging, then uniformly stirring in an open mill, and then rolling at the temperature of 60 ℃ to obtain a second-section mixing film;
(4) Rolling out a sheet: putting the two-stage mixed roll into a calender for calendering and discharging, wherein the calendering temperature is 55 ℃, the thickness of the calendered film is 2mm, and cooling and coiling the calendered film to obtain the calendered film;
(5) Vulcanizing the rubber plate: vulcanizing by a drum vulcanizing machine: the method adopts a multi-layer film laminating process, the rolled films are separated by a guide roller before entering a main drum to prevent adhesion and air inclusion, the tension of each layer of the rolled films is independently controlled, the tension of the multi-layer rolled films is kept consistent, the temperature of the main drum is 168 ℃, the auxiliary heating temperature of a steel belt is 185 ℃, and the multi-layer rolled film is obtained by cooling and coiling after vulcanization.
Example 3
A chlorinated polyethylene rubber composition comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber CPE135B,10 parts of magnesium oxide, 0.2 part of anti-aging agent NBC,40 parts of white carbon black, 40 parts of heavy calcium carbonate, 3.0 parts of flow promoter R-300V,25 parts of TOTM,2.5 parts of thiadiazole derivative ECHO A and 1 part of accelerator 808.
The preparation method of the chlorinated polyethylene rubber composition for the vulcanized chlorinated polyethylene rubber plate comprises the following preparation steps:
(1) Plasticizing: plasticizing chlorinated polyethylene rubber in an open mill for 5 times by adopting a thin pass method, and coating rollers for discharging sheets to obtain chlorinated polyethylene plasticized rubber;
(2) First-stage mixing: adding chlorinated polyethylene plasticizing rubber, magnesium oxide, an anti-aging agent NBC and R-300V into an internal mixer, mixing for 30 seconds, adding white carbon black, heavy calcium carbonate and TOTM, mixing for 480 seconds at the mixing temperature of 110 ℃, discharging, uniformly mixing in an open mixer, then discharging, standing for more than 8 hours to obtain a section of mixed rubber sheet;
(3) And (3) second-stage mixing: putting the parked first-stage mixed rubber sheet into an internal mixer, adding a cross-linking agent ECHO & A and an accelerant 808, mixing for 120 seconds, discharging, then uniformly smashing and mixing in an open mill, and then rolling at the temperature of 65 ℃ to obtain a second-stage mixed rubber sheet;
(4) Rolling out a sheet: putting the two-stage mixed roll film into a calender for calendering and discharging, wherein the calendering temperature is 60 ℃, the thickness of the calendered film is 2.5mm, and cooling and coiling to obtain a calendered film;
(5) Vulcanizing the rubber plate: vulcanizing by a drum vulcanizing machine: the method adopts a multi-layer film laminating process, the rolled films are separated by a guide roller before entering a main drum to prevent adhesion and air inclusion, the tension of each layer of the rolled films is independently controlled, the tension of the multi-layer rolled films is kept consistent, the temperature of the main drum is 170 ℃, the auxiliary heating temperature of a steel belt is 190 ℃, and the multi-layer rolled film is obtained by cooling and coiling after vulcanization.
Example 4
A chlorinated polyethylene rubber composition comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber CPE135B,5 parts of magnesium oxide, 1 part of calcium stearate, 1 part of barium stearate, 0.4 part of an anti-aging agent NBC,55 parts of carbon black N990, 80 parts of zinc borate decahydrate, 2.0 parts of a flow aid R-300V,35 parts of DOP,2 parts of thiadiazole derivative ECHO & A and 3 parts of an accelerator 808.
The preparation method of the chlorinated polyethylene rubber composition for the vulcanized chlorinated polyethylene rubber plate comprises the following preparation steps:
(1) Plasticizing: plasticizing chlorinated polyethylene rubber in an open mill for 5 times by adopting a thin pass method, and wrapping the chlorinated polyethylene rubber by a roller to obtain chlorinated polyethylene plasticized rubber;
(2) First-stage mixing: adding chlorinated polyethylene plasticizing glue, magnesium oxide, calcium stearate, barium stearate, an anti-aging agent NBC and R-300V into an internal mixer, mixing for 30 seconds, adding carbon black N990, zinc borate decahydrate and DOP, mixing for 330 seconds at the mixing temperature of 115 ℃, discharging, uniformly stirring in an open mill, then discharging, and standing for more than 8 hours to obtain a section of mixed rubber sheet;
(3) And (2) two-stage mixing: putting the parked first-section mixing rubber sheet into an internal mixer, adding a cross-linking agent ECHO & A and an accelerant 808, mixing for 120 seconds, discharging, then uniformly mixing in an open mill, and then rolling down at the temperature of 60 ℃ to obtain a second-section mixing rubber roll;
(4) Rolling out a sheet: putting the two-stage mixed roll into a calender for calendering and sheet discharging, wherein the calendering temperature is 55 ℃, the thickness of the calendered sheet is 2.5mm, and cooling and coiling the calendered sheet to obtain a calendered sheet;
(5) Vulcanizing the rubber plate: vulcanizing by a flat vulcanizing machine: pre-compounding the multi-layer rolled films into a semi-finished product (a tower-shaped section is formed by stacking from top to bottom) with the thickness of 110-120% and the width of 90-95% of the finished product by using a film compounding machine, wherein the weight of a single semi-finished product is 102-107% of the weight of the finished product, the vulcanization temperature is 168 ℃, the pot mouth temperature is less than or equal to 95 ℃, the vulcanization pressure is 3.0MPa, the vulcanization time is 12min, and cooling, trimming and cutting at fixed length are carried out after vulcanization to obtain the finished product.
Comparative example 1
In the formulation of the chlorinated polyethylene rubber composition in comparative example 1, no flow aid R-300V was added, and the other components and the preparation method were the same as in example 1.
Comparative example 2
In comparative example 2, a chlorinated polyethylene rubber composition is provided, comprising the following components in parts by weight: 100 parts of chlorinated polyethylene rubber, 20 parts of heat stabilizer, 0.05 part of anti-aging agent, 50 parts of reinforcing agent and 20 parts of
Inorganic filler, 8 parts of flow assistant R-300V,10 parts of plasticizer, 2 parts of crosslinking agent and 1 part of auxiliary crosslinking agent. The compounding ingredients were prepared in the same manner as in example 1, except that the compounding ingredients were used in a different ratio from those in examples 1 to 4 of the present invention.
The rubber sheets prepared in examples 1 to 4 and comparative examples 1 to 2 were subjected to basic data tests, and the test data are shown in table 1:
TABLE 1 test parameters of examples and comparative examples of vulcanized chlorinated polyethylene rubber sheets
As can be seen from the data in table 1, the performance of examples 1-4 is significantly better than comparative examples 1 and 2. The flow assistant-compound fatty acid R-300V has obvious internal lubrication effect on a rubber mixing system, greatly improves the demolding property and the mechanical property of the plate in the rubber plate vulcanization process, can prepare the rubber plate with smooth and flat surface and extremely small shrinkage deformation through a drum type vulcanizing machine and a flat plate vulcanizing machine, has good mechanical property, heat resistance, aging resistance, flame retardance and oil resistance of a finished product, and can correspondingly replace expensive special rubber plates. The proportion of the ingredients is continuously and perfectly summarized by the inventor on the basis of a large number of experiments, and the ingredients in the proportion range can act synergistically, so that the high-quality rubber sheet material with excellent performance and good appearance can be prepared.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A chlorinated polyethylene rubber composition characterized by: the paint comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber, 2-15 parts of heat stabilizer, 0.1-0.5 part of anti-aging agent, 10-60 parts of reinforcing agent, 20-80 parts of inorganic filler, 2-6 parts of flow promoter, 10-35 parts of plasticizer, 2-5 parts of cross-linking agent and 1-5 parts of auxiliary cross-linking agent;
the flow auxiliary agent is compound fatty acid R-300V.
2. A chlorinated polyethylene rubber composition according to claim 1, characterized in that: the paint comprises the following components in parts by weight: 100 parts of chlorinated polyethylene rubber, 4-13 parts of heat stabilizer, 0.2-0.4 part of anti-aging agent, 15-55 parts of reinforcing agent, 20-50 parts of inorganic filler, 2-4 parts of flow promoter, 10-25 parts of plasticizer, 2-4 parts of cross-linking agent and 1-3 parts of auxiliary cross-linking agent.
3. A chlorinated polyethylene rubber composition according to claim 1 or 2, characterized in that: the chlorinated polyethylene rubber is CPE135B; and/or
The heat stabilizer is at least one of calcium stearate, barium stearate and magnesium oxide.
4. A chlorinated polyethylene rubber composition according to claim 1 or 2, characterized in that: the anti-aging agent is N, N' -dibutyl dithiocarbamic acid nickel.
5. A chlorinated polyethylene rubber composition according to claim 1 or 2, characterized in that: the reinforcing agent is at least one of carbon black N660, carbon black N774, carbon black N990 and white carbon black; and/or
The inorganic filler is at least one of light calcium carbonate, heavy calcium carbonate, barium sulfate and zinc borate decahydrate.
6. A chlorinated polyethylene rubber composition according to claim 1 or 2, characterized in that: the plasticizer is at least one of dioctyl phthalate, tricresyl phosphate, trioctyl trimellitate and chlorinated paraffin; and/or
The cross-linking agent is one of bis (1-methyl-1-phenethyl) peroxide, 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane and thiadiazole derivative ECHO.A; and/or
The assistant crosslinking agent is one of N, N' -m-phenylene maleimide and an accelerator 808.
7. A vulcanized chlorinated polyethylene rubber sheet prepared from the chlorinated polyethylene rubber composition according to any one of claims 1 to 6.
8. A method for producing a vulcanized chlorinated polyethylene rubber sheet, which is used for producing the vulcanized chlorinated polyethylene rubber sheet according to claim 7, wherein the method comprises the following steps: the preparation method comprises the following preparation steps:
(1) Plasticizing: plasticizing the chlorinated polyethylene rubber by adopting a thin pass method to obtain a chlorinated polyethylene plasticized rubber;
(2) First-stage mixing: adding the chlorinated polyethylene plasticizing rubber, the heat stabilizer, the anti-aging agent, the flow assistant, the reinforcing agent, the inorganic filler and the plasticizer into an internal mixer to be mixed for a period of 6-10 min at the mixing temperature of 110-120 ℃, discharging, uniformly mixing in an open mill, then discharging, placing, and obtaining a section of mixed rubber sheet;
(3) And (3) second-stage mixing: carrying out two-stage mixing on the first-stage mixing rubber sheet, the cross-linking agent and the auxiliary cross-linking agent in an internal mixer for 90-120 s, discharging, then uniformly smashing and mixing in an open mill, and then rolling to obtain a two-stage mixing film;
(4) Rolling out a sheet: putting the two-stage mixing film into a calender for calendering and sheet discharging, cooling and then coiling to obtain a calendered film;
(5) Vulcanizing the rubber plate: vulcanizing, cooling and coiling the calendered film on a drum vulcanizer by adopting a multilayer film laminating process; or vulcanizing by a flat vulcanizing machine, cooling and cutting edges to obtain the vulcanized chlorinated polyethylene rubber sheet.
9. The method for preparing a vulcanized chlorinated polyethylene rubber sheet according to claim 8, wherein the method comprises the following steps: when the calendered films are vulcanized by a drum vulcanizer in the step (5), separating multiple calendered films by guide rollers before entering a main drum, wherein the sum of the thicknesses of the multiple calendered films is 103-105% of the thickness of a finished product, the temperature of the main drum of the drum vulcanizer is 165-170 ℃, steel belt auxiliary heating is adopted, the temperature of the steel belt auxiliary heating is 180-190 ℃, and the finished product is the vulcanized chlorinated polyethylene rubber plate finally obtained in the step (5); and/or
When the calendered films are vulcanized by a flat vulcanizing machine in the step (5), a film compounding machine is adopted to pre-compound the multiple layers of calendered films into a semi-finished product with the thickness of 110% -120% of the thickness of a finished product and the width of 90% -95% of the width of the finished product, the weight of a single semi-finished product is 102% -107% of the weight of the finished product, the vulcanization temperature is 165 ℃ -170 ℃, the pot mouth temperature of the flat vulcanizing machine is less than or equal to 95 ℃, the vulcanization pressure is 2.5 MPa-4.0 MPa, the vulcanization time is 8 min-15 min, and the finished product is the vulcanized chlorinated polyethylene rubber sheet finally obtained in the step (5).
10. The method for preparing a vulcanized chlorinated polyethylene rubber sheet according to claim 8, wherein: the plasticizing frequency in the step (1) is 3-5; and/or
The parking time in the step (2) is at least 8h; and/or
The temperature is 55-65 ℃ when the coil is fed in the step (3); and/or
In the step (4), the calendering temperature is 50-60 ℃, and when the drum vulcanizer is used for vulcanization, the thickness of the calendered film is 1-2.5 mm; when the flat vulcanizing machine is used for vulcanizing, the thickness of the calendering film is 2.0 mm-3.5 mm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03163146A (en) * | 1989-11-22 | 1991-07-15 | Tosoh Corp | Chlorinated polyethylene rubber composition |
| CN106633441A (en) * | 2016-11-04 | 2017-05-10 | 南京利德东方橡塑科技有限公司 | High-temperature-resistant CPE rubber composition, preparation method, application and application product thereof |
| WO2020011005A1 (en) * | 2018-07-13 | 2020-01-16 | 杭州星庐科技有限公司 | Chlorine-containing rubber composition, and application thereof and preparation method therefor |
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- 2022-12-30 CN CN202211724458.2A patent/CN115975302A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03163146A (en) * | 1989-11-22 | 1991-07-15 | Tosoh Corp | Chlorinated polyethylene rubber composition |
| CN106633441A (en) * | 2016-11-04 | 2017-05-10 | 南京利德东方橡塑科技有限公司 | High-temperature-resistant CPE rubber composition, preparation method, application and application product thereof |
| WO2020011005A1 (en) * | 2018-07-13 | 2020-01-16 | 杭州星庐科技有限公司 | Chlorine-containing rubber composition, and application thereof and preparation method therefor |
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