CN116355299A - Standard reference glue material and preparation method and application thereof - Google Patents
Standard reference glue material and preparation method and application thereof Download PDFInfo
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- CN116355299A CN116355299A CN202310381108.9A CN202310381108A CN116355299A CN 116355299 A CN116355299 A CN 116355299A CN 202310381108 A CN202310381108 A CN 202310381108A CN 116355299 A CN116355299 A CN 116355299A
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- 239000000463 material Substances 0.000 title claims abstract description 73
- 239000003292 glue Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 229920001971 elastomer Polymers 0.000 claims abstract description 99
- 239000005060 rubber Substances 0.000 claims abstract description 98
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 40
- 238000012360 testing method Methods 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 19
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 28
- 238000004073 vulcanization Methods 0.000 claims description 23
- 244000043261 Hevea brasiliensis Species 0.000 claims description 22
- 239000005062 Polybutadiene Substances 0.000 claims description 22
- 229920003052 natural elastomer Polymers 0.000 claims description 22
- 229920001194 natural rubber Polymers 0.000 claims description 22
- 229920002857 polybutadiene Polymers 0.000 claims description 22
- 239000012744 reinforcing agent Substances 0.000 claims description 21
- 239000013543 active substance Substances 0.000 claims description 18
- 230000003712 anti-aging effect Effects 0.000 claims description 17
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 12
- 238000000748 compression moulding Methods 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- -1 3, 5-di-tert-butyl-4-hydroxyphenyl Chemical group 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000007670 refining Methods 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 7
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 7
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 6
- ZNRLMGFXSPUZNR-UHFFFAOYSA-N 2,2,4-trimethyl-1h-quinoline Chemical compound C1=CC=C2C(C)=CC(C)(C)NC2=C1 ZNRLMGFXSPUZNR-UHFFFAOYSA-N 0.000 claims description 6
- XOUQAVYLRNOXDO-UHFFFAOYSA-N 2-tert-butyl-5-methylphenol Chemical compound CC1=CC=C(C(C)(C)C)C(O)=C1 XOUQAVYLRNOXDO-UHFFFAOYSA-N 0.000 claims description 6
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 239000004973 liquid crystal related substance Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- IUJLOAKJZQBENM-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)-2-methylpropan-2-amine Chemical compound C1=CC=C2SC(SNC(C)(C)C)=NC2=C1 IUJLOAKJZQBENM-UHFFFAOYSA-N 0.000 claims description 6
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 6
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000008117 stearic acid Substances 0.000 claims description 6
- 229960002447 thiram Drugs 0.000 claims description 6
- 239000011787 zinc oxide Substances 0.000 claims description 6
- BUZICZZQJDLXJN-UHFFFAOYSA-N 3-azaniumyl-4-hydroxybutanoate Chemical compound OCC(N)CC(O)=O BUZICZZQJDLXJN-UHFFFAOYSA-N 0.000 claims description 3
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003508 Dilauryl thiodipropionate Substances 0.000 claims description 3
- 235000019304 dilauryl thiodipropionate Nutrition 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 claims description 3
- 125000001501 propionyl group Chemical group O=C([*])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 239000002656 Distearyl thiodipropionate Substances 0.000 claims 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims 1
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 claims 1
- 235000019305 distearyl thiodipropionate Nutrition 0.000 claims 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims 1
- 238000005299 abrasion Methods 0.000 abstract description 38
- 230000007774 longterm Effects 0.000 abstract description 7
- 239000003921 oil Substances 0.000 description 16
- 238000007599 discharging Methods 0.000 description 8
- 238000001514 detection method Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000010998 test method Methods 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 238000007689 inspection Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000004636 vulcanized rubber Substances 0.000 description 4
- 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 3
- 238000013112 stability test Methods 0.000 description 3
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012031 short term test Methods 0.000 description 2
- JSTCPNFNKICNNO-UHFFFAOYSA-N 4-nitrosophenol Chemical class OC1=CC=C(N=O)C=C1 JSTCPNFNKICNNO-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- PXJJSXABGXMUSU-UHFFFAOYSA-N disulfur dichloride Chemical compound ClSSCl PXJJSXABGXMUSU-UHFFFAOYSA-N 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- WORCCYVLMMTGFR-UHFFFAOYSA-M loxoprofen sodium Chemical compound [Na+].C1=CC(C(C([O-])=O)C)=CC=C1CC1C(=O)CCC1 WORCCYVLMMTGFR-UHFFFAOYSA-M 0.000 description 1
- 125000005439 maleimidyl group Chemical class C1(C=CC(N1*)=O)=O 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000009666 routine test Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 150000003673 urethanes Chemical class 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
- C08L21/00—Compositions of unspecified rubbers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/56—Investigating resistance to wear or abrasion
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
Abstract
The invention provides a standard reference glue material, a preparation method and application thereof. The standard reference rubber material comprises a rubber base material, an ethylene-vinyl acetate copolymer, a vulcanizing agent, naphthenic oil and tire powder; wherein, based on 100 parts by weight of the total rubber substrate, the content of the ethylene-vinyl acetate copolymer is 5-20 parts, the content of the vulcanizing agent is 2-5 parts, the content of the naphthenic oil is 15-30 parts, and the content of the tire powder is 50-100 parts. The standard reference glue material has low abrasion mass loss, small relative expansion uncertainty and good abrasion test uniformity and stability (including long-term stability and short-term transportation stability).
Description
Technical Field
The invention relates to a standard reference glue material and a preparation method and application thereof, in particular to a standard reference glue material applied to wear resistance test of a roller type abrasion machine method and a preparation method and application thereof, belonging to the field of standard materials.
Background
During the process of wearing the shoes, the soles are subjected to friction force, so that abrasion is generated. Abrasion is the interaction of materials with other objects or the impact of hard particles such as sand. The wear resistance of the sole directly affects the service life of the footwear product, and is an important technical index for measuring the quality grade of the footwear product. Thus, the performance of sole wear tests is one of the most important routine tests for the production and inspection of footwear products.
The existing wear resistance detection methods of the shoe products mainly comprise 5 types of wear resistance detection methods, including a whole shoe wear resistance detection method, an Alcron wear machine method, a roller wear machine method, a NBS (National bureau of standard) wear test machine method and a Lanbine test machine method, and the 5 types of test methods have different test principles and characteristics. The roller type abrasion machine abrasion test is also called DIN (Deutsches Institut Normung) abrasion test, is an important international and domestic test method, and can be widely applied to abrasion performance tests of related products of rubber elastomer materials at home and abroad, such as products of soles, tires, conveyor belts, rubber strips and the like.
The DIN abrasion test has the advantages of stable test process, simple and quick operation, small sample size, non-repeated friction test track and the like, and the test error caused by the operation of test equipment and personnel can be effectively reduced because the method adopts the standard reference glue (namely the standard reference glue for the abrasion test of the roller abrasion machine method) in the test process. The standard reference glue materials used in the related laboratories at home and abroad at present are all BAM standard glue produced by German Federal materials detection institute.
As the number of detection mechanisms and detection requirements rise at high speed, the demands for test consumables and standard samples are also increasing. DIN abrasion test has wide application field and larger demand, and leads to the gradual supply and undersupply of BAM standard glue. However, in practice, the product has the defects of poor uniformity, easy frosting and the like. Therefore, the independent development of the wear-resistant test standard reference glue of the roller type abrasion machine method has higher social value and good economic benefit, not only can promote the implementation and implementation of related character standards, but also can improve the accuracy and result traceability of the detection mechanism to the wear-resistant test of the roller type abrasion machine method.
Disclosure of Invention
Problems to be solved by the invention
In view of the technical problems existing in the prior art, the invention firstly provides a standard reference glue material. The standard reference glue material has low abrasion mass loss, small relative expansion uncertainty, good abrasion test uniformity and long-term and short-term test stability.
Furthermore, the invention also provides a preparation method of the standard reference gel material, which is simple and feasible, is easy to obtain raw materials and is suitable for mass production.
Solution for solving the problem
The invention relates to a standard reference rubber material, which comprises a rubber base material, an ethylene-vinyl acetate copolymer, a vulcanizing agent, naphthenic oil and tire powder; wherein, the liquid crystal display device comprises a liquid crystal display device,
the total mass portion of the rubber base material is 100 portions, the content of the ethylene-vinyl acetate copolymer is 5-20 portions, the content of the vulcanizing agent is 2-5 portions, the content of the naphthenic oil is 15-30 portions, and the content of the tire powder is 50-100 portions.
The standard reference rubber material comprises a rubber substrate, wherein the rubber substrate comprises butadiene rubber and natural rubber; preferably, the butadiene rubber content is 40-60 parts and the natural rubber content is 40-60 parts based on 100 parts of the total mass of the rubber substrate.
The standard reference glue material provided by the invention further comprises one or more than two of a reinforcing agent, an active agent, an anti-aging agent and an accelerator; preferably, the content of the reinforcing agent is 50-75 parts, the content of the active agent is 5-15 parts, the content of the accelerator is 2-5 parts, and the content of the anti-aging agent is 2-15 parts based on 100 parts by weight of the total mass of the rubber substrate.
The standard reference glue material according to the invention, wherein the reinforcing agent comprises calcium carbonate and/or white carbon black.
The standard reference glue material according to the invention, wherein the active agent comprises one or more of diethylene glycol, polyethylene glycol, stearic acid, magnesium oxide and zinc oxide.
The standard reference glue material according to the invention, wherein the anti-aging agent comprises one or a combination of more than two of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 1, 2-bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 4' -thio-bis (6-tert-butyl-3-methylphenol), thiodistearyl dipropionate and dilauryl thiodipropionate.
The standard reference glue material according to the invention, wherein the accelerator comprises one or a combination of more than two of N-cyclohexyl-2-benzothiazole sulfenamide, N-tertiary butyl-2-benzothiazole sulfenamide, 2' -dibenzothiazyl disulfide, tetramethylthiuram monosulfide, 2-mercaptobenzothiazole and tetramethylthiuram disulfide.
The invention also provides a preparation method of the standard reference gel material, which comprises the step of mixing the components of the standard reference gel material.
The preparation method according to the invention comprises the following steps:
mixing the components of the standard reference rubber material, and then mixing to obtain a mixed rubber;
refining the rubber compound to obtain a rubber compound;
and carrying out compression molding vulcanization molding on the mixed rubber sheet to obtain the standard reference rubber material.
The invention also provides application of the standard reference glue material in the roller type abrasion machine abrasion resistance test.
ADVANTAGEOUS EFFECTS OF INVENTION
The standard reference glue material has low abrasion mass loss, small relative expansion uncertainty and good abrasion test uniformity and stability (including long-term stability and short-term transportation stability).
Furthermore, the preparation method of the standard reference gel material is simple and feasible, the raw materials are easy to obtain, and the standard reference gel material is suitable for mass production.
Detailed Description
Various exemplary embodiments, features and aspects of the invention are described in detail below. The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better illustration of the invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In other instances, well known methods, procedures, means, equipment and steps have not been described in detail so as not to obscure the present invention.
Unless otherwise indicated, all units used in this specification are units of international standard, and numerical values, ranges of values, etc. appearing in the present invention are understood to include systematic errors unavoidable in industrial production.
In the present specification, the meaning of "can" includes both the meaning of performing a certain process and the meaning of not performing a certain process.
Reference throughout this specification to "some specific/preferred embodiments," "other specific/preferred embodiments," "an embodiment," and so forth, means that a particular element (e.g., feature, structure, property, and/or characteristic) described in connection with the embodiment is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the elements may be combined in any suitable manner in the various embodiments.
In the present specification, the numerical range indicated by the term "numerical value a to numerical value B" means a range including the end point numerical value A, B.
In the present specification, when "normal temperature" and "room temperature" are used, the temperature may be 10 to 25 ℃.
<First aspect>
A first aspect of the present invention provides a standard reference rubber material comprising a rubber substrate, an ethylene-vinyl acetate copolymer, a vulcanizing agent, a naphthenic oil, and a tire powder; wherein, the liquid crystal display device comprises a liquid crystal display device,
the total mass portion of the rubber base material is 100 portions, the content of the ethylene-vinyl acetate copolymer is 5-20 portions, the content of the vulcanizing agent is 2-5 portions, the content of the naphthenic oil is 15-30 portions, and the content of the tire powder is 50-100 portions.
The standard reference glue material has low abrasion mass loss, small relative expansion uncertainty, good abrasion test uniformity and long-term and short-term test stability. Specifically:
the rubber substrate of the present invention preferably includes butadiene rubber and natural rubber;
the inventors of the present invention found that natural rubber has excellent elasticity, insulation, water-blocking properties, but is generally required to be used with other rubbers and to improve its use properties due to its poor aging resistance and weather resistance. Butadiene rubber has excellent low temperature resistance, wear resistance, low heat generation and dynamic mechanical property compared with natural rubber. The blending of the natural rubber and the butadiene rubber not only can effectively improve the ageing and wear resistance of the product, but also can improve the low temperature resistance effect of the product. Therefore, butadiene rubber and natural rubber are preferably used as the rubber base material of the present invention.
Preferably, the butadiene rubber is contained in an amount of 40 to 60 parts by weight based on 100 parts by weight of the total rubber base material, for example: 42 parts, 45 parts, 48 parts, 50 parts, 52 parts, 55 parts, etc.; the content of the natural rubber is 40 to 60 parts, for example: 42 parts, 45 parts, 48 parts, 50 parts, 52 parts, 55 parts, etc. The inventor discovers that when the content of butadiene rubber is 40-60 parts and the content of natural rubber is 40-60 parts, the effects of the butadiene rubber and the natural rubber can be effectively exerted, and the butadiene rubber is suitable for being used as a rubber substrate of the application.
In the invention, the ethylene-vinyl acetate copolymer is used for further improving the cohesiveness and processability of butadiene rubber and natural rubber, so as to achieve better thermodynamic compatibility effect, thereby obtaining the standard reference rubber material with excellent performance.
Preferably, the ethylene-vinyl acetate copolymer is contained in an amount of 5 to 20 parts by weight based on 100 parts by weight of the total rubber substrate, for example: 8 parts, 10 parts, 12 parts, 15 parts, 18 parts, etc.; when the content of the ethylene-vinyl acetate copolymer is 5 to 20 parts, the adhesion and processability between butadiene rubber and natural rubber can be further effectively improved.
In the present invention, the vulcanized rubber is obtained by using a vulcanizing agent. The vulcanizing agent is not particularly limited, and may be one commonly used in the art. Specifically, in the present invention, the vulcanizing agent is contained in an amount of 2 to 5 parts by weight based on 100 parts by weight of the total rubber substrate, for example: 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, etc.; when the content of the vulcanizing agent is 2 to 5 parts, it is more advantageous to obtain the desired vulcanized rubber.
In general, vulcanizing agents include inorganic vulcanizing agents and organic vulcanizing agents. The inorganic vulcanizing agent comprises sulfur, sulfur monochloride, selenium, tellurium and the like. The organic vulcanizing agent includes sulfur-containing accelerators (such as accelerator TMTD), organic peroxides (such as benzoyl peroxide), quinone oxime compounds, polysulfide polymers, urethanes, maleimide derivatives, and the like. In the present invention, sulfur is preferably used as the vulcanizing agent in view of not introducing other impurities.
In the invention, the standard reference rubber material further contains naphthenic oil, and the content of the naphthenic oil is 15-30 parts based on 100 parts by weight of the total mass of the rubber substrate, for example: 18 parts, 20 parts, 22 parts, 25 parts, 28 parts, etc. The naphthenic oil of the invention can be used for reducing the Mooney viscosity to improve the in-mold flow, thereby better molding. When the content of the naphthenic oil is 15 to 30 parts, the work efficiency of the naphthenic oil can be most effectively exerted.
Further, the standard reference rubber material of the present invention further contains a tire powder, the content of the tire powder is 50 to 100 parts by weight based on 100 parts by weight of the total mass of the rubber base material, for example: 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, 90 parts, 95 parts, etc. The present invention reduces the cost by using the tire powder, and naturally, the more the cost is added, the lower the cost is, but the basic physical properties and moldability of the rubber are ensured. In addition, the inventor of the present invention found that the addition of tire powder to the standard reference rubber material of the present application can improve the wear uniformity and aging resistance of the standard reference rubber material. When the content of the tire powder is 50-100 parts, the efficacy can be most effectively exerted.
In some specific embodiments, the standard reference glue material further comprises one or a combination of more than two of a reinforcing agent, an active agent, an anti-aging agent and an accelerator; preferably, the content of the reinforcing agent is 50-75 parts, the content of the active agent is 5-15 parts, the content of the accelerator is 2-5 parts, and the content of the anti-aging agent is 2-15 parts based on 100 parts by weight of the total mass of the rubber substrate.
As for the reinforcing agent, the reinforcing agent is used to play a role of filling and reinforcing, so that the mechanical strength of rubber can be improved. Further, in the present invention, the content of the reinforcing agent is 50 to 75 parts by weight based on 100 parts by weight of the total of the rubber base material, for example: 52 parts, 55 parts, 58 parts, 60 parts, 62 parts, 65 parts, 68 parts, 70 parts, 72 parts, etc. When the content of the reinforcing agent is 50-75 parts, the mechanical strength of the rubber can be effectively improved. Specifically, the reinforcing agent comprises calcium carbonate and/or white carbon black. The white carbon black is also called precipitation method hydrated silicon dioxide, white smoke and the like.
For the active agent, the active agent can increase the activity of a vulcanization accelerator, improve the vulcanization speed and vulcanization efficiency of the rubber material and improve the chemical substance of the vulcanized rubber performance. Further, the content of the active agent is 5 to 15 parts by weight based on 100 parts by weight of the total rubber substrate, for example: 7 parts, 9 parts, 11 parts, 13 parts, etc. When the content of the active agent is 5-15 parts, the active agent can better play a role, improve the vulcanization activity and improve the smoothness and texture of the vulcanized rubber surface.
Specifically, the active agent comprises one or more than two of diethylene glycol, polyethylene glycol, stearic acid, magnesium oxide and zinc oxide.
As for the anti-aging agent, the anti-aging agent is adopted to prevent the aging of rubber, prolong the service life of rubber products and ensure that the standard reference rubber material has excellent anti-aging effect. Further, the content of the antioxidant is 2 to 15 parts by weight based on 100 parts by weight of the total rubber substrate, for example: 4 parts, 5 parts, 7 parts, 9 parts, 11 parts, 13 parts, etc. When the content of the anti-aging agent is 2-15 parts, the aging of rubber can be effectively prevented, and the service life of the rubber product is prolonged.
Further, the anti-aging agent comprises one or a combination of more than two of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 1, 2-bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 4' -thiobis (6-tert-butyl-3-methylphenol), thiodistearyl dipropionate and dilauryl thiodipropionate.
The accelerator can accelerate the crosslinking reaction of the sizing material, shorten the vulcanization time, reduce the vulcanization temperature and reduce the dosage of the vulcanizing agent. Further, in the present invention, the accelerator is contained in an amount of 2 to 5 parts by weight based on 100 parts by weight of the total rubber base material, for example: 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, etc.; when the content of the accelerator is 2-5 parts, the vulcanization acceleration effect can be exerted higher, and the scorching safety is ensured.
Specifically, the accelerator comprises one or more than two of N-cyclohexyl-2-benzothiazole sulfenamide, N-tertiary butyl-2-benzothiazole sulfenamide, 2' -dibenzothiazyl disulfide, tetramethyl thiuram monosulfide, 2-mercaptobenzothiazole and tetramethyl thiuram disulfide.
<Second aspect>
A second aspect of the present invention provides a method of preparing a standard reference gel material according to the first aspect of the present invention, comprising the step of mixing the components of the standard reference gel material.
In some specific embodiments, the method of making comprises:
mixing the components of the standard reference rubber material, and then mixing to obtain a mixed rubber;
refining the rubber compound to obtain a rubber compound;
and carrying out compression molding vulcanization molding on the mixed rubber sheet to obtain the standard reference rubber material.
Specifically, the preparation method comprises the following steps:
(1) Mixing natural rubber, butadiene rubber, ethylene-vinyl acetate copolymer, other optional additives and vulcanizing agent to obtain a mixed rubber;
(2) Refining the rubber compound to obtain a rubber compound;
(3) And carrying out compression molding vulcanization molding on the mixed rubber sheet to obtain the standard reference rubber material.
Specifically, the preparation method of the standard reference glue material comprises the following steps:
(1) Banburying: plasticating the natural rubber and the butadiene rubber in an internal mixer, wherein the internal mixing temperature is controlled within the range of 55-65 ℃ for 3-5min, and the rotating speed of the internal mixer is 60-70rpm; adding ethylene-vinyl acetate copolymer, banburying for 5-8min, and controlling the banburying temperature within 75-90 ℃; adding the reinforcing agent for 2-3 times, wherein the time interval of each addition is 1-3min, and mixing for 5-10min until the reinforcing agent is uniformly dispersed; adding tire powder, mixing for 3-5min until the tire powder is uniformly dispersed, and controlling the banburying temperature within 90 ℃; adding an active agent and an anti-aging agent, and mixing for 2-3min; the banburying temperature is controlled within the range of 55-65 ℃; adding naphthenic oil, mixing for 2-3min, adding vulcanizing agent and accelerator, mixing for 2-3min, and discharging to obtain a mixed rubber;
(2) Refining: mixing the mixed rubber on an open mill, standing for 24 hours after discharging the mixed rubber to obtain a mixed rubber sheet;
(3) Compression molding: and (3) putting the mixed rubber sheet into a flat vulcanizing machine for compression molding and vulcanization molding, wherein the vulcanization temperature is 150-160 ℃, and the vulcanization time is 3-5min, so that the wear-resisting test standard reference rubber of the roller type abrasion machine method is obtained, and the sample size is 181mm multiplied by 8mm.
Furthermore, the invention also provides application of the standard reference glue material in the roller type abrasion machine abrasion resistance test.
Examples
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. 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.
Example 1
The composition (mass ratio) is: 55 parts of natural rubber, 45 parts of butadiene rubber, 15 parts of ethylene-vinyl acetate copolymer, 50 parts of white carbon black, 10 parts of calcium carbonate, 80 parts of tire powder, 15 parts of naphthenic oil, 5 parts of zinc oxide, 1.0 part of polyethylene glycol, 1.0 part of stearic acid, 2.5 parts of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 2 parts of 2,2' -dibenzothiazyl disulfide, 0.5 part of tetramethylthiuram disulfide, 0.6 part of N-tertiary butyl-2-benzothiazole sulfenamide and 3 parts of sulfur.
The preparation method comprises the following steps:
(1) Banburying: plasticating the natural rubber and the butadiene rubber in an internal mixer, wherein the internal mixing temperature is controlled to be 60 ℃, the time is 5min, and the rotating speed of the internal mixer is 60rpm; adding ethylene-vinyl acetate copolymer, banburying for 5min, and controlling the banburying temperature within 90 ℃; adding the reinforcing agent for 3 times, wherein the time interval of each addition is 2min, and mixing for 8min until the reinforcing agent is uniformly dispersed; adding tire powder, mixing for 5min until the tire powder is uniformly dispersed, and controlling the banburying temperature within 90 ℃; adding an active agent and an anti-aging agent, and mixing for 3min; the banburying temperature is controlled within the range of 60 ℃; adding naphthenic oil, mixing for 3min, adding a vulcanizing agent and an accelerator, mixing for 2min, and discharging to obtain a mixed rubber;
(2) Refining: mixing the mixed rubber on an open mill, standing for 24 hours after discharging the mixed rubber to obtain a mixed rubber sheet;
(3) Compression molding: and (3) putting the mixed rubber sheet into a flat vulcanizing machine for compression molding and vulcanization molding, wherein the vulcanization temperature is 155 ℃, the vulcanization time is 5min, and the wear-resisting test standard reference rubber of the roller type abrasion machine method is obtained, and the sample size is 181mm multiplied by 8mm.
Example 2
The composition (mass ratio) is: 50 parts of natural rubber, 50 parts of butadiene rubber, 15 parts of ethylene-vinyl acetate copolymer, 50 parts of white carbon black, 10 parts of calcium carbonate, 85 parts of tire powder, 15 parts of naphthenic oil, 5 parts of zinc oxide, 1.0 part of polyethylene glycol, 1.0 part of stearic acid, 2.5 parts of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 2 parts of 2,2' -dibenzothiazyl disulfide, 0.5 part of tetramethylthiuram disulfide, 0.6 part of N-tertiary butyl-2-benzothiazole sulfenamide and 3 parts of sulfur.
The preparation method comprises the following steps:
(1) Banburying: plasticating the natural rubber and the butadiene rubber in an internal mixer, wherein the internal mixing temperature is controlled to be 60 ℃, the time is 4min, and the rotating speed of the internal mixer is 60rpm; adding ethylene-vinyl acetate copolymer, banburying for 5min, and controlling the banburying temperature within 90 ℃; adding the reinforcing agent for 3 times, wherein the time interval of each addition is 2min, and mixing for 8min until the reinforcing agent is uniformly dispersed; adding tire powder, mixing for 5min until the tire powder is uniformly dispersed, and controlling the banburying temperature within 90 ℃; adding an active agent and an anti-aging agent, and mixing for 3min; the banburying temperature is controlled within the range of 60 ℃; adding naphthenic oil, mixing for 3min, adding a vulcanizing agent and an accelerator, mixing for 2min, and discharging to obtain a mixed rubber;
(2) Refining: mixing the mixed rubber on an open mill, standing for 24 hours after discharging the mixed rubber to obtain a mixed rubber sheet;
(3) Compression molding: and (3) putting the mixed rubber sheet into a flat vulcanizing machine for compression molding and vulcanization molding, wherein the vulcanization temperature is 155 ℃, the vulcanization time is 5min, and the wear-resisting test standard reference rubber of the roller type abrasion machine method is obtained, and the sample size is 181mm multiplied by 8mm.
Example 3
The composition (mass ratio) is: 45 parts of natural rubber, 55 parts of butadiene rubber, 17 parts of ethylene-vinyl acetate copolymer, 50 parts of white carbon black, 15 parts of calcium carbonate, 85 parts of tire powder, 20 parts of naphthenic oil, 5 parts of zinc oxide, 1.0 part of polyethylene glycol, 1.0 part of stearic acid, 2.5 parts of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 2 parts of 2,2' -dibenzothiazyl disulfide, 0.5 part of tetramethylthiuram disulfide, 0.6 part of N-tertiary butyl-2-benzothiazole sulfenamide and 3 parts of sulfur.
The preparation method comprises the following steps:
(1) Banburying: plasticating the natural rubber and the butadiene rubber in an internal mixer, wherein the internal mixing temperature is controlled within the range of 60 ℃ for 3min, and the rotating speed of the internal mixer is 60rpm; adding ethylene-vinyl acetate copolymer, banburying for 5min, and controlling the banburying temperature within 90 ℃; adding the reinforcing agent for 3 times, wherein the time interval of each addition is 2min, and mixing for 10min until the reinforcing agent is uniformly dispersed; adding tire powder, mixing for 5min until the tire powder is uniformly dispersed, and controlling the banburying temperature within 90 ℃; adding an active agent and an anti-aging agent, and mixing for 3min; the banburying temperature is controlled within the range of 60 ℃; adding naphthenic oil, mixing for 3min, adding a vulcanizing agent and an accelerator, mixing for 2min, and discharging to obtain a mixed rubber;
(2) Refining: mixing the mixed rubber on an open mill, standing for 24 hours after discharging the mixed rubber to obtain a mixed rubber sheet;
(3) Compression molding: and (3) putting the mixed rubber sheet into a flat vulcanizing machine for compression molding and vulcanization molding, wherein the vulcanization temperature is 155 ℃, the vulcanization time is 4min, and the wear-resisting test standard reference rubber of the roller type abrasion machine method is obtained, and the sample size is 181mm multiplied by 8mm.
Performance testing
1. Abrasion loss of quality test, hardness test
The standard reference gel materials prepared in examples 1 to 3 were cut into cylindrical samples with a diameter of 16mm according to the requirements of the test sample in GB/T9867-2008, 10 samples were taken, and the abrasion mass loss was tested by using the test method (non-rotating test method) of the standard reference gel No. 1 specified in GB/T9867-2008, and the hardness was tested by using GB/T3903.4-2017. Wherein the model of the abrasion tester is high-speed rail GT-7012-D, the model of the Shore A hardness tester is Shanghai six-diamond LX-A, and various performance indexes are shown in table 1.
Table 1 standard reference glue material abrasion and hardness test results
As can be seen from Table 1, the abrasion mass loss range of the reference adhesive for the abrasion testing standard of the roller type abrasion machine method prepared by the invention is (180-200) mg, the Shore hardness A also meets the requirements of GB/T9867-2008, and samples have good abrasion uniformity. The sample prepared by the formulation and process of example 3 had a loss of abrasion mass closer to the standard requirements and the uniformity was optimal.
2. Stability test
The sample prepared in the embodiment 3 of the invention is subjected to short-term stability and long-term stability (36 months) inspection, the test method is carried out according to the test method (non-rotating sample method) of the standard reference glue No. 1 specified in GB/T9867-2008, the inspection data are subjected to data statistics processing by adopting a T-test method, and the statistics of the inspection result shows that the T calculated values are smaller than the T critical value, so that the sample has good short-term stability and long-term stability, and the test results are shown in tables 2 and 3.
TABLE 2 short term stability test results
TABLE 3 long-term stability test results
3. Application testing
10 unit samples were randomly cut from the samples prepared in example 3 of the present invention and the BAM standard gel, respectively, and each sample was tested by method A (non-rotating test sample method) in GB/T9867-2008, and the results are shown in Table 4 below.
Table 4 comparison test results
| Sample numbering | Example 3 sample | BAM standard adhesive |
| SAM-001 | 202 | 211 |
| SAM-002 | 202 | 196 |
| SAM-003 | 207 | 201 |
| SAM-004 | 197 | 195 |
| SAM-005 | 206 | 201 |
| SAM-006 | 199 | 210 |
| SAM-007 | 201 | 208 |
| SAM-008 | 207 | 192 |
| SAM-009 | 196 | 213 |
| SAM-010 | 198 | 200 |
| Average value (mg) | 201 | 203 |
| RSD(％) | 2.03 | 3.63 |
The comparison test results in Table 4 show that the standard relative deviation of the prepared sample is slightly lower than that of BAM standard glue, and the prepared sample has good uniformity and stability and can completely replace the BAM standard glue.
It should be noted that, although the technical solution of the present invention is described in specific examples, those skilled in the art can understand that the present invention should not be limited thereto.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. The terminology used herein was chosen in order to best explain the principles of the embodiments, the practical application, or the technical improvements in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. A standard reference rubber material, which is characterized by comprising a rubber base material, an ethylene-vinyl acetate copolymer, a vulcanizing agent, naphthenic oil and tire powder; wherein, the liquid crystal display device comprises a liquid crystal display device,
the total mass portion of the rubber base material is 100 portions, the content of the ethylene-vinyl acetate copolymer is 5-20 portions, the content of the vulcanizing agent is 2-5 portions, the content of the naphthenic oil is 15-30 portions, and the content of the tire powder is 50-100 portions.
2. The standard reference rubber material of claim 1, wherein the rubber substrate comprises butadiene rubber and natural rubber; preferably, the butadiene rubber is contained in an amount of 40 to 60 parts by weight and the natural rubber is contained in an amount of 40 to 60 parts by weight based on 100 parts by weight of the total rubber base material.
3. The standard reference glue material according to claim 1 or 2, further comprising one or a combination of two or more of a reinforcing agent, an active agent, an anti-aging agent, and an accelerator; preferably, the content of the reinforcing agent is 50-75 parts, the content of the active agent is 5-15 parts, the content of the accelerator is 2-5 parts, and the content of the anti-aging agent is 2-15 parts based on 100 parts by weight of the total mass of the rubber substrate.
4. A standard reference gel material according to claim 3, wherein the reinforcing agent comprises calcium carbonate and/or white carbon black.
5. The standard reference gel material of claim 3 or 4, wherein the active agent comprises one or a combination of more than two of diethylene glycol, polyethylene glycol, stearic acid, magnesium oxide, zinc oxide.
6. The standard reference gel material of any one of claims 3-5, wherein the anti-aging agent comprises one or a combination of two or more of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 1, 2-bis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester, 4' -thiobis (6-tert-butyl-3-methylphenol), distearyl thiodipropionate, and dilauryl thiodipropionate.
7. The standard reference gel material of any one of claims 3-6, wherein the accelerator comprises one or a combination of two or more of N-cyclohexyl-2-benzothiazole sulfenamide, N-t-butyl-2-benzothiazole sulfenamide, 2' -dibenzothiazyl disulfide, tetramethylthiuram monosulfide, 2-mercaptobenzothiazole, tetramethylthiuram disulfide.
8. A method of preparing a standard reference gel material according to any one of claims 1 to 7, comprising the step of mixing the components of the standard reference gel material.
9. The method of manufacturing according to claim 8, characterized in that the method of manufacturing comprises:
mixing the components of the standard reference rubber material, and then mixing to obtain a mixed rubber;
refining the rubber compound to obtain a rubber compound;
and carrying out compression molding vulcanization molding on the mixed rubber sheet to obtain the standard reference rubber material.
10. Use of a standard reference gel material according to any one of claims 1-7 in a roller abrader wear test.
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