CN116904017A - Polyurethane vulcanized rubber and preparation method and application thereof - Google Patents
Polyurethane vulcanized rubber and preparation method and application thereof Download PDFInfo
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- CN116904017A CN116904017A CN202310859712.8A CN202310859712A CN116904017A CN 116904017 A CN116904017 A CN 116904017A CN 202310859712 A CN202310859712 A CN 202310859712A CN 116904017 A CN116904017 A CN 116904017A
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- acrylic resin
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- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 43
- 239000004814 polyurethane Substances 0.000 title claims abstract description 43
- 239000004636 vulcanized rubber Substances 0.000 title claims abstract description 38
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 45
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 45
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011347 resin Substances 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000013543 active substance Substances 0.000 claims abstract description 24
- 239000006229 carbon black Substances 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 24
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011593 sulfur Substances 0.000 claims abstract description 23
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 23
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 21
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 21
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000008117 stearic acid Substances 0.000 claims abstract description 21
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 26
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 24
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 24
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 24
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 19
- QTKPMCIBUROOGY-UHFFFAOYSA-N 2,2,2-trifluoroethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)F QTKPMCIBUROOGY-UHFFFAOYSA-N 0.000 claims description 15
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 8
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 26
- 229920001971 elastomer Polymers 0.000 description 9
- 239000011737 fluorine Substances 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- 239000000806 elastomer Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 238000004073 vulcanization Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920003225 polyurethane elastomer Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/46—Bases; Cases
- H01R13/52—Dustproof, splashproof, drip-proof, waterproof, or flameproof cases
- H01R13/523—Dustproof, splashproof, drip-proof, waterproof, or flameproof cases for use under water
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses polyurethane vulcanized rubber, a preparation method and application thereof, and relates to the technical field of cables, wherein the vulcanized rubber comprises the following preparation raw materials in parts by weight: 100 parts of MPU, 5 to 8 parts of coumarone resin, 1 to 2 parts of fluorosilicone modified acrylic resin, 0.5 to 0.6 part of stearic acid, 2 to 3 parts of active agent, 2 to 3 parts of sulfur, 30 to 40 parts of carbon black and 4 to 8 parts of accelerator. Therefore, the invention leads the vulcanized rubber to have excellent mechanical property and water resistance by mutual compatibility of the MPU, the coumarone resin and the fluorosilicone modified acrylic resin.
Description
Technical Field
The invention belongs to the technical field of cables, and particularly relates to polyurethane vulcanized rubber and a preparation method and application thereof.
Background
The watertight cable is an indispensable key component such as a submarine, a sonar, a submarine sound transducer, an underwater robot and the like, is mainly used in an underwater ship power supply system, is a bridge for connecting a power supply and electric equipment, and is required to ensure the reliability of electrifying under normal conditions and the safety of the submarine under accident conditions, so that the watertight cable is required to have good tensile property and reliable watertight performance, is convenient for connecting equipment and the power supply in the underwater power supply system, meets the requirements of deepwater power supply of the naval power supply system due to the development of the watertight cable, and can prevent seawater from leaking from the inside of a cable structure to other cabins or entering into a parameter equipment instrument when the cable is damaged due to local accidents in the use process, and ensure the watertight bulkhead safety; vulcanized rubber seals are arranged between joints of underwater cables and watertight heads.
The sealing effect of the urethane vulcanized rubber has great influence on water tightness; while the hydrolysis resistance of polyurethanes in the related art is relatively poor.
Disclosure of Invention
The present invention is directed to a polyurethane curing adhesive that overcomes at least one of the problems and deficiencies set forth in the background art discussed above.
The second aspect of the invention provides a preparation method of the polyurethane vulcanized rubber.
The third aspect of the invention provides the use of the polyurethane vulcanizate described above.
The first aspect of the invention provides polyurethane vulcanized rubber, which comprises the following preparation raw materials in parts by weight:
100 parts of MPU, 5 to 8 parts of coumarone resin, 1 to 2 parts of fluorosilicone modified acrylic resin, 0.5 to 0.6 part of stearic acid, 2 to 3 parts of active agent, 2 to 3 parts of sulfur, 30 to 40 parts of carbon black and 4 to 8 parts of accelerator.
According to one of the technical schemes of the polyurethane vulcanized rubber, the polyurethane vulcanized rubber at least comprises the following components
The beneficial effects are that:
MPU (mixing polyurethane rubber) is selected, and has the characteristics of excellent wear resistance, solvent resistance, cold resistance and high strength; the coumarone resin has thermoplastic property, and the rubber has good cohesiveness, is easier to vulcanize and process by adding the coumarone resin, can improve the dispersion degree of sulfur in the rubber material, and improves the tensile strength and hardness of the elastomer when improving the vulcanization uniformity degree; the fluorine-silicon modified resin is introduced with fluorine element containing polarity, so that the interfacial tension between elastomer components is effectively reduced, interfacial compatibility is promoted, and the uniformity of granulation and vulcanization is improved; meanwhile, the fluorine-silicon element has better hydrophobicity, and can greatly improve the water resistance.
Therefore, the invention leads the vulcanized rubber to have excellent mechanical property and water resistance by mutual compatibility of the MPU, the coumarone resin and the fluorosilicone modified acrylic resin.
According to some embodiments of the invention, the MPU is named SW70 of Shanxi Changzhi chemical plant.
According to some embodiments of the invention, the active agent is NH-2 (Shanghai double crown chemical Co., ltd.).
According to some embodiments of the invention, the carbon black is N330.
According to some embodiments of the invention, the accelerator consists of accelerator D (diphenyl guanidine), accelerator DM (dibenzothiazyl disulfide) and accelerator PZ (zinc dimethyldithiocarbamate).
According to some embodiments of the invention, the mass ratio of the accelerator D, the accelerator DM and the accelerator PZ is 1:1 to 1.5:1 to 1.5.
According to some embodiments of the present invention, the fluorosilicone-modified acrylic resin comprises the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 10-20 parts of trifluoroethyl methacrylate, 5-7 parts of methacryloxypropyl trimethoxy silane, 50-60 parts of propylene glycol methyl ether and 2-3 parts of benzoyl peroxide.
The invention also discloses a preparation method of the polyurethane vulcanized rubber, which comprises the following steps:
plasticizing MPU, adding coumarone resin, fluorosilicone modified acrylic resin, stearic acid, active agent, sulfur, carbon black and promoter, and mixing.
According to some embodiments of the present invention, the method for preparing the fluorosilicone-modified acrylic resin includes the steps of:
mixing butyl acrylate, trifluoroethyl methacrylate, methacryloxypropyl trimethoxysilane and propylene glycol methyl ether to obtain a first mixture;
and mixing the first mixture with benzoyl peroxide for reaction.
According to some embodiments of the present invention, the method for preparing the fluorosilicone-modified acrylic resin includes the steps of:
s1, mixing butyl acrylate, trifluoroethyl methacrylate, methacryloxypropyl trimethoxysilane and propylene glycol methyl ether to prepare a first mixture;
s2, mixing the first mixture with benzoyl peroxide for reaction.
According to some embodiments of the invention, the temperature of the mixing in step S1 is 100 ℃ to 110 ℃.
According to some embodiments of the invention, the mixing time in step S1 is 1h to 2h.
According to some embodiments of the invention, the temperature of the reaction in step S2 is 110 ℃ to 120 ℃.
According to some embodiments of the invention, the reaction time in step S2 is 2h to 3h.
According to some embodiments of the invention, the plasticizing temperature is 80 ℃ to 100 ℃.
According to some embodiments of the invention, the plasticizing time is 3min to 5min.
According to some embodiments of the invention, the temperature of the mixing is 150 ℃ to 160 ℃.
According to some embodiments of the invention, the mixing time is from 10 minutes to 20 minutes.
According to some embodiments of the invention, the pressure of the mixing is between 10MPa and 15MPa.
The third aspect of the invention discloses application of the polyurethane vulcanized rubber in preparation of watertight connectors.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
In the description of the present invention, the descriptions of the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In the embodiment of the invention, the MPU brand is SW70 of Shanxi Changzhi chemical plant.
In an embodiment of the invention the active agent is NH-2.
In the embodiment of the invention, the carbon black is N330.
The accelerator in the embodiment of the invention consists of an accelerator D, an accelerator DM and an accelerator PZ according to the mass ratio of 1:1:1.2.
Example 1
The embodiment is a polyurethane vulcanized rubber, which is prepared from the following raw materials in parts by weight:
100 parts of MPU, 7 parts of coumarone resin, 1.8 parts of fluorosilicone modified acrylic resin, 0.6 part of stearic acid, 3 parts of active agent, 2 parts of sulfur, 30 parts of carbon black and 6.4 parts of accelerator.
The fluorosilicone modified acrylic resin in the embodiment comprises the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 12 parts of trifluoroethyl methacrylate, 6 parts of methacryloxypropyl trimethoxysilane, 60 parts of propylene glycol methyl ether and 3 parts of benzoyl peroxide.
The preparation method of the fluorosilicone modified acrylic resin in the embodiment comprises the following steps:
s1, mixing butyl acrylate, trifluoroethyl methacrylate, methacryloxypropyl trimethoxysilane and propylene glycol methyl ether, and then preserving heat at 110 ℃ for 1.5 hours to prepare a first mixture.
S2, mixing 1/2 of benzoyl peroxide in the formula amount with the first mixture, and then preserving heat for 1h at 117 ℃ to prepare a second mixture.
S3, mixing 1/2 of benzoyl peroxide in the formula amount with the second mixture, and then preserving heat for 1.5h at 125 ℃.
The preparation method of the polyurethane vulcanized rubber in the embodiment comprises the following steps:
plasticizing MPU at 80deg.C for 3min; mixing coumarone resin, fluorosilicone modified acrylic resin, stearic acid, active agent, sulfur, carbon black and promoter, and mixing at 150 deg.c for 15min at 15MPa.
Example 2
The embodiment is a polyurethane vulcanized rubber, which is prepared from the following raw materials in parts by weight:
100 parts of MPU, 5 parts of coumarone resin, 2 parts of fluorosilicone modified acrylic resin, 0.6 part of stearic acid, 3 parts of active agent, 2 parts of sulfur, 40 parts of carbon black and 6.4 parts of accelerator.
The fluorosilicone modified acrylic resin in the embodiment comprises the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 10 parts of trifluoroethyl methacrylate, 7 parts of methacryloxypropyl trimethoxysilane, 60 parts of propylene glycol methyl ether and 3 parts of benzoyl peroxide.
The preparation method of the polyurethane vulcanized rubber and the preparation method of the fluorosilicone-modified acrylic resin in this example were carried out with reference to example 1.
Example 3
The embodiment is a polyurethane vulcanized rubber, which is prepared from the following raw materials in parts by weight:
100 parts of MPU, 7 parts of coumarone resin, 1.5 parts of fluorosilicone modified acrylic resin, 0.5 part of stearic acid, 2 parts of active agent, 3 parts of sulfur, 32 parts of carbon black and 6.4 parts of accelerator.
The fluorosilicone modified acrylic resin in the embodiment comprises the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 20 parts of trifluoroethyl methacrylate, 5 parts of methacryloxypropyl trimethoxysilane, 60 parts of propylene glycol methyl ether and 3 parts of benzoyl peroxide.
The preparation method of the polyurethane vulcanized rubber and the preparation method of the fluorosilicone-modified acrylic resin in this example were carried out with reference to example 1.
Example 4
The embodiment is a polyurethane vulcanized rubber, which is prepared from the following raw materials in parts by weight:
100 parts of MPU, 6 parts of coumarone resin, 1.2 parts of fluorosilicone modified acrylic resin, 0.6 part of stearic acid, 2.3 parts of active agent, 2.5 parts of sulfur, 32 parts of carbon black and 6.4 parts of accelerator.
The fluorosilicone modified acrylic resin in the embodiment comprises the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 14 parts of trifluoroethyl methacrylate, 7 parts of methacryloxypropyl trimethoxysilane, 60 parts of propylene glycol methyl ether and 3 parts of benzoyl peroxide.
The preparation method of the polyurethane vulcanized rubber and the preparation method of the fluorosilicone-modified acrylic resin in this example were carried out with reference to example 1.
Example 5
The embodiment is a polyurethane vulcanized rubber, which is prepared from the following raw materials in parts by weight:
100 parts of MPU, 8 parts of coumarone resin, 1 part of fluorosilicone modified acrylic resin, 0.5 part of stearic acid, 3 parts of active agent, 2 parts of sulfur, 35 parts of carbon black and 6.4 parts of accelerator.
The fluorosilicone modified acrylic resin in the embodiment comprises the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 17 parts of trifluoroethyl methacrylate, 5 parts of methacryloxypropyl trimethoxysilane, 60 parts of propylene glycol methyl ether and 3 parts of benzoyl peroxide.
The preparation method of the polyurethane vulcanized rubber and the preparation method of the fluorosilicone-modified acrylic resin in this example were carried out with reference to example 1.
Comparative example 1
The comparative example is a polyurethane vulcanized rubber, which consists of the following preparation raw materials in parts by weight:
100 parts of MPU, 8 parts of coumarone resin, 0.5 part of stearic acid, 3 parts of active agent, 2 parts of sulfur, 35 parts of carbon black and 6.4 parts of accelerator.
The preparation method of the polyurethane vulcanized rubber in the comparative example comprises the following steps:
plasticizing MPU at 80deg.C for 3min; mixing coumarone resin, stearic acid, active agent, sulfur, carbon black and promoter, and mixing at 150deg.C for 15min (mixing pressure of 15 MPa).
Comparative example 2
The comparative example is a polyurethane vulcanized rubber, which consists of the following preparation raw materials in parts by weight:
100 parts of MPU, 8 parts of coumarone resin, 1 part of fluorine modified acrylic resin, 0.5 part of stearic acid, 3 parts of active agent, 2 parts of sulfur, 35 parts of carbon black and 6.4 parts of accelerator.
The fluorine modified acrylic resin in the comparative example consists of the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 17 parts of trifluoroethyl methacrylate, 60 parts of propylene glycol methyl ether and 3 parts of benzoyl peroxide.
The preparation method of the fluorine modified acrylic resin in the comparative example comprises the following steps:
s1, mixing butyl acrylate, trifluoroethyl methacrylate and propylene glycol methyl ether, and then preserving heat at 110 ℃ for 1.5 hours to prepare a first mixture.
S2, mixing 1/2 of benzoyl peroxide in the formula amount with the first mixture, and then preserving heat for 1h at 117 ℃ to prepare a second mixture.
S3, mixing 1/2 of benzoyl peroxide in the formula amount with the second mixture, and then preserving heat for 1.5h at 125 ℃.
The preparation method of the polyurethane vulcanized rubber in the comparative example comprises the following steps:
plasticizing MPU at 80deg.C for 3min; mixing coumarone resin, fluorine modified acrylic resin, stearic acid, an active agent, sulfur, carbon black and an accelerator, and then mixing for 15min at 150 ℃ (mixing pressure is 15 MPa).
Comparative example 3
The comparative example is a polyurethane vulcanized rubber, which consists of the following preparation raw materials in parts by weight:
100 parts of MPU, 8 parts of coumarone resin, 1 part of silicon modified acrylic resin, 0.5 part of stearic acid, 3 parts of active agent, 2 parts of sulfur, 35 parts of carbon black and 6.4 parts of accelerator.
The silicon modified acrylic resin in the comparative example consists of the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 5 parts of methacryloxypropyl trimethoxysilane, 60 parts of propylene glycol methyl ether and 3 parts of benzoyl peroxide.
The preparation method of the silicon modified acrylic resin in the comparative example comprises the following steps:
s1, mixing butyl acrylate, methacryloxypropyl trimethoxysilane and propylene glycol methyl ether, and then preserving heat at 110 ℃ for 1.5 hours to prepare a first mixture.
S2, mixing 1/2 of benzoyl peroxide in the formula amount with the first mixture, and then preserving heat for 1h at 117 ℃ to prepare a second mixture.
S3, mixing 1/2 of benzoyl peroxide in the formula amount with the second mixture, and then preserving heat for 1.5h at 125 ℃.
The preparation method of the polyurethane vulcanized rubber in the comparative example comprises the following steps:
plasticizing MPU at 80deg.C for 3min; mixing coumarone resin, silicon modified acrylic resin, stearic acid, active agent, sulfur, carbon black and accelerator, and mixing at 150deg.C for 15min (mixing pressure of 15 MPa).
Comparative example 4
The comparative example is a polyurethane vulcanized rubber, which consists of the following preparation raw materials in parts by weight:
100 parts of MPU, 8 parts of coumarone resin, 1 part of acrylic resin, 0.5 part of stearic acid, 3 parts of active agent, 2 parts of sulfur, 35 parts of carbon black and 6.4 parts of accelerator.
The modified acrylic resin in the comparative example consists of the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 60 parts of propylene glycol methyl ether and 3 parts of benzoyl peroxide.
The preparation method of the fluorosilicone modified acrylic resin in the comparative example comprises the following steps:
s1, mixing butyl acrylate and propylene glycol methyl ether, and then preserving heat for 1.5 hours at 110 ℃ to prepare a first mixture.
S2, mixing 1/2 of benzoyl peroxide in the formula amount with the first mixture, and then preserving heat for 1h at 117 ℃ to prepare a second mixture.
S3, mixing 1/2 of benzoyl peroxide in the formula amount with the second mixture, and then preserving heat for 1.5h at 125 ℃.
The preparation method of the polyurethane vulcanized rubber in the comparative example comprises the following steps:
plasticizing MPU at 80deg.C for 3min; mixing coumarone resin, acrylic resin, stearic acid, active agent, sulfur, carbon black and promoter, and mixing at 150deg.C for 15min (mixing pressure of 15 MPa).
Comparative example 5
The comparative example is a polyurethane vulcanized rubber, which consists of the following preparation raw materials in parts by weight:
100 parts of MPU, 4 parts of coumarone resin, 0.5 part of fluorosilicone modified acrylic resin, 0.5 part of stearic acid, 3 parts of active agent, 2 parts of sulfur, 35 parts of carbon black and 6.4 parts of accelerator.
The fluorosilicone modified acrylic resin in the comparative example consists of the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 17 parts of trifluoroethyl methacrylate, 5 parts of methacryloxypropyl trimethoxysilane, 60 parts of propylene glycol methyl ether and 3 parts of benzoyl peroxide.
The preparation method of the fluorosilicone modified acrylic resin in the comparative example comprises the following steps:
s1, mixing butyl acrylate, trifluoroethyl methacrylate, methacryloxypropyl trimethoxysilane and propylene glycol methyl ether, and then preserving heat at 110 ℃ for 1.5 hours to prepare a first mixture.
S2, mixing 1/2 of benzoyl peroxide in the formula amount with the first mixture, and then preserving heat for 1h at 117 ℃ to prepare a second mixture.
S3, mixing 1/2 of benzoyl peroxide in the formula amount with the first mixture, and then preserving heat for 1.5h at 125 ℃.
The preparation method of the polyurethane vulcanized rubber in the comparative example comprises the following steps:
plasticizing MPU at 80deg.C for 3min; mixing coumarone resin, fluorosilicone modified acrylic resin, stearic acid, active agent, sulfur, carbon black and promoter, and mixing at 150 deg.c for 15min at 15MPa.
The mechanical properties and the water resistance of the composite elastomer materials obtained in each example and comparative example were tested according to the method described in the national standard GB/T2951 test method for mechanical physical Properties of Cable.
The tensile properties were measured according to GB/T528, type I specimens having a thickness of 2mm and a tensile cross-section width of 6mm and a tensile speed of 500mm/min.
Elongation at break, measured at room temperature.
Hydrolysis resistance was characterized by the rate of change of tensile strength of the test samples after being cooked at 100 ℃ for 168 hours. The results of the polyurethane vulcanizate performance test of inventive examples 1-5 and comparative examples 1-5 are shown in Table 1.
TABLE 1 results of polyurethane vulcanizate performance test of inventive examples 1-5 and comparative examples 1-5
In summary, the present invention selects MPU (compounded polyurethane rubber) which has excellent abrasion resistance, solvent resistance, cold resistance and high strength; the coumarone resin has thermoplastic property, and the rubber has good cohesiveness, is easier to vulcanize and process by adding the coumarone resin, can improve the dispersion degree of sulfur in the rubber material, and improves the tensile strength and hardness of the elastomer when improving the vulcanization uniformity degree; the fluorine-silicon modified resin is introduced with fluorine element containing polarity, so that the interfacial tension between elastomer components is effectively reduced, interfacial compatibility is promoted, and the uniformity of granulation and vulcanization is improved; meanwhile, the fluorine-silicon element has better hydrophobicity, and can greatly improve the water resistance. Therefore, the invention leads the vulcanized rubber to have excellent mechanical property and hydrolysis resistance by mutual compatibility of the MPU, the coumarone resin and the fluorosilicone modified acrylic resin.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.
Claims (10)
1. The polyurethane vulcanized rubber is characterized by comprising the following preparation raw materials in parts by weight:
100 parts of MPU, 5 to 8 parts of coumarone resin, 1 to 2 parts of fluorosilicone modified acrylic resin, 0.5 to 0.6 part of stearic acid, 2 to 3 parts of active agent, 2 to 3 parts of sulfur, 30 to 40 parts of carbon black and 4 to 8 parts of accelerator.
2. The polyurethane curing adhesive of claim 1, wherein the active agent is NH-2.
3. The polyurethane vulcanizate of claim 1, wherein the carbon black is N330.
4. The polyurethane curing adhesive of claim 1, wherein the accelerator consists of accelerator D, accelerator DM and accelerator PZ.
5. The polyurethane curing adhesive according to claim 5, wherein the mass ratio of the accelerator D, the accelerator DM and the accelerator PZ is 1:1-1.5:1-1.5.
6. The polyurethane vulcanized rubber according to claim 1, wherein the fluorosilicone modified acrylic resin comprises the following preparation raw materials in parts by weight:
100 parts of butyl acrylate, 10-20 parts of trifluoroethyl methacrylate, 5-7 parts of methacryloxypropyl trimethoxy silane, 50-60 parts of propylene glycol methyl ether and 2-3 parts of benzoyl peroxide.
7. A process for preparing a polyurethane vulcanizate according to any one of claims 1 to 6, comprising the steps of:
plasticizing MPU, adding coumarone resin, fluorosilicone modified acrylic resin, stearic acid, active agent, sulfur, carbon black and promoter, and mixing.
8. The method according to claim 7, wherein the method for producing the fluorosilicone-modified acrylic resin comprises the steps of:
s1, mixing butyl acrylate, trifluoroethyl methacrylate, methacryloxypropyl trimethoxysilane and propylene glycol methyl ether to prepare a first mixture;
s2, mixing the first mixture with benzoyl peroxide for reaction.
9. The method of claim 7, wherein the temperature of the mixing is 150 ℃ to 160 ℃.
10. Use of a polyurethane vulcanizate according to any one of claims 1 to 6 for the preparation of watertight connectors.
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