CN113563639A - Light-colored solid silane coupling agent - Google Patents
Light-colored solid silane coupling agent Download PDFInfo
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- CN113563639A CN113563639A CN202110835947.4A CN202110835947A CN113563639A CN 113563639 A CN113563639 A CN 113563639A CN 202110835947 A CN202110835947 A CN 202110835947A CN 113563639 A CN113563639 A CN 113563639A
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- 239000006087 Silane Coupling Agent Substances 0.000 title claims abstract description 71
- 239000007787 solid Substances 0.000 title claims abstract description 41
- 229920001971 elastomer Polymers 0.000 claims abstract description 53
- 239000005060 rubber Substances 0.000 claims abstract description 53
- 239000006229 carbon black Substances 0.000 claims abstract description 34
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 22
- 239000010456 wollastonite Substances 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 5
- 239000002131 composite material Substances 0.000 abstract description 27
- 239000000463 material Substances 0.000 abstract description 19
- 238000002156 mixing Methods 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 11
- 238000005096 rolling process Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000003756 stirring Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000005303 weighing Methods 0.000 abstract description 4
- 239000007822 coupling agent Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 20
- 238000007599 discharging Methods 0.000 description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 12
- 238000004073 vulcanization Methods 0.000 description 11
- 239000004594 Masterbatch (MB) Substances 0.000 description 8
- 244000043261 Hevea brasiliensis Species 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 229920003052 natural elastomer Polymers 0.000 description 7
- 229920001194 natural rubber Polymers 0.000 description 7
- 229920003048 styrene butadiene rubber Polymers 0.000 description 7
- 235000021355 Stearic acid Nutrition 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 230000003712 anti-aging effect Effects 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 description 6
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 6
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 6
- 239000008117 stearic acid Substances 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- 239000011787 zinc oxide Substances 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 239000004200 microcrystalline wax Substances 0.000 description 4
- 235000019808 microcrystalline wax Nutrition 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000002174 Styrene-butadiene Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000012744 reinforcing agent Substances 0.000 description 3
- 101100434170 Oryza sativa subsp. japonica ACR2.1 gene Proteins 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 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
- 230000020169 heat generation Effects 0.000 description 2
- 229920006247 high-performance elastomer Polymers 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010423 industrial mineral Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010734 process oil Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- FBBATURSCRIBHN-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyldisulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSCCC[Si](OCC)(OCC)OCC FBBATURSCRIBHN-UHFFFAOYSA-N 0.000 description 1
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/548—Silicon-containing compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/06—Copolymers with styrene
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 belongs to the technical field of coupling agents, and relates to a light-colored solid silane coupling agent which is prepared by mixing 10 parts by weight of wollastonite and 1-10 parts by weight of liquid silane coupling agent and uniformly stirring, can equivalently replace the conventional solid silane coupling agent taking carbon black as a carrier, and prepares a rubber product by adopting a conventional rubber material preparation process; the light-colored solid silane coupling agent is prepared by taking wollastonite as a carrier, can be used for producing light-colored rubber materials, and solves the problem of pollution of the conventional solid silane coupling agent taking carbon black as a carrier to the color of the rubber materials; the composite material prepared by the method has the advantages of improving the stress at definite elongation, tensile strength and tensile product coefficient, reducing the rolling resistance to some extent, reducing the environmental protection problem in the production process, reducing the production cost, facilitating the weighing and feeding of the silane coupling agent and having good market application value in the rubber industry field.
Description
The technical field is as follows:
the invention belongs to the technical field of coupling agents, and relates to a light-colored solid silane coupling agent which takes wollastonite as a carrier and can be used for preparing high-performance rubber products.
Background art:
in the rubber industry, inorganic filler is used for filling and reinforcing composite materials, so that the performance of the composite materials can be effectively improved, and white carbon black and carbon black are commonly used reinforcing agents. Compared with the traditional reinforcing agent carbon black in the rubber industry, the rubber reinforced by the white carbon black has the characteristics of small hysteresis loss, low rolling resistance, excellent wet skid resistance and the like. However, the surface of the white carbon black has a large amount of hydroxyl groups, so that the white carbon black shows good hydrophilicity, so that the white carbon black has poor compatibility with hydrophobic rubber matrix materials, and meanwhile, the large amount of hydroxyl groups contained on the surface of the white carbon black are easy to agglomerate under the action of hydrogen bonds, so that the dispersibility of the white carbon black in the rubber matrix is poor, and the processing and the service performance of the composite material are seriously influenced. Therefore, the white carbon black needs to be modified to improve the bonding property with rubber and improve the dispersibility in a rubber matrix, and a common method is to add a silane coupling agent into a composite material for surface modification.
The silane coupling agent is a widely used modifier, one end of the molecule of the silane coupling agent can react with the filler, and the other end of the molecule of the silane coupling agent can react with a rubber molecular chain, so that the silane coupling agent plays a role in chemical bridging between rubber and the filler, and further improves the comprehensive performance of natural rubber, and therefore, the silane coupling agent is widely applied to the rubber industry.
Silane coupling agents are generally in a liquid state, so that weighing and feeding are inconvenient in the mixing process of rubber materials, hydrolysis self-polymerization reaction is easy to occur when the silane coupling agents meet water, the product quality is seriously affected, and the problems of color change and precipitation caused by excessive impurities are easy to remain in the preparation process, so that the silane coupling agents are often required to be granulated.
The solid silane coupling agent obtained after granulation treatment can facilitate weighing and feeding in the mixing process of rubber materials, achieves the purpose of being put into an internal mixer at one time, does not need to be slowly fed, can effectively prevent self-hydrolytic self-polymerization reaction in the mixing process, and is favorable for uniform dispersion of the silane coupling agent.
At present, the widely used granulation process is to mix equal mass of carbon black and silane coupling agent and then stir them. However, after the solid silane coupling agent particles granulated by the carbon black are added into the rubber material, the rubber material almost inevitably presents black due to the strong blackness and coloring power of the carbon black, and meanwhile, the preparation process of the carbon black has the problems of large energy consumption and serious pollution, and the rubber material filled with the carbon black has the defects of inevitable increase of heat generation and reduction of wet skid resistance, does not accord with the trend of reduction of the carbon black dosage in the formula of the green tire rubber material, and is not suitable for the future development direction of green manufacturing.
Wollastonite is a natural industrial mineral with the molecular formula of CaSiO3The color is generally white, the whiteness is higher, the reserves are rich, the environment-friendly and nontoxic, the heat stability, the acid and alkali resistance, the chemical corrosion resistance and the insulativity are good, the composite material can be used as a filler and a reinforcing agent of a high polymer composite material, and the rubber composite material filled with wollastonite also has lower rolling resistance. Therefore, the light-colored solid silane coupling agent is prepared by taking wollastonite as a carrier, so that the silane coupling agent is coated on the surface of the wollastonite, the performance of the rubber composite material is improved, and the development prospect is good.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and develops and designs a light-color solid silane coupling agent taking wollastonite as a carrier, and prepares a solid silane coupling agent by taking the wollastonite with higher whiteness and large length-diameter ratio as the carrier, so as to prepare a high-performance rubber product.
In order to achieve the purpose, the light-color solid silane coupling agent is prepared by mixing 10 parts by mass of wollastonite and 1-10 parts by mass of liquid silane coupling agent and uniformly stirring.
The whiteness of the wollastonite is 50-90, the median particle diameter D50 is 1-20 mu m, the length-diameter ratio is 1-20:1, and the wollastonite has a needle-like, fibrous and bundle-like structure; silane coupling agents include, but are not limited to, Si69, i.e., bis (γ -triethoxysilylpropyl) tetrasulfide, Si75, i.e., bis- [3- (triethoxysilyl) propyl ] -disulfide, KH-550, i.e., γ -aminopropyltriethoxysilane.
The light-colored solid silane coupling agent can equivalently replace the conventional solid silane coupling agent which takes carbon black as a carrier, and a rubber product is prepared by adopting the conventional rubber compound preparation process.
Compared with the prior art, the method has the advantages that the wollastonite is used as the carrier to prepare the light-colored solid silane coupling agent, so that the method can be used for producing light-colored rubber materials, and the problem of pollution of the conventional solid silane coupling agent using carbon black as the carrier to the color of the rubber materials is solved; the composite material prepared by the method has the advantages of improving the stress at definite elongation, tensile strength and tensile product coefficient, reducing the rolling resistance to some extent, reducing the environmental protection problem in the production process, reducing the production cost, facilitating the weighing and feeding of the silane coupling agent and having good market application value in the rubber industry field.
The specific implementation mode is as follows:
the invention is further illustrated by the following examples.
Example 1:
the light-colored solid silane coupling agent related to the embodiment is prepared from 5 parts by weight of a silane coupling agent, wherein the whiteness is 85, the median particle diameter D50 is 3.08 mu m, and the length-diameter ratio is 10: 1 wollastonite and 3 parts by mass of liquid Si69, and stirring the mixture evenly to prepare the silicon dioxide coating,
the formula for preparing the composite material by using the light-colored solid silane coupling agent comprises the following components in parts by weight: 2025 parts of natural rubber STR, 150275 parts of styrene butadiene rubber SBR, 75 parts of white carbon black, 16 parts of light-colored solid silane coupling agent, 70025 parts of process oil V, 2 parts of stearic acid, 2 parts of zinc oxide, 40202 parts of anti-aging agent, 1.5 parts of microcrystalline wax, 1.2 parts of accelerator DPG, 2.5 parts of accelerator CZ and 1.25 parts of sulfur; the specific process for preparing the composite material comprises the following steps:
first-stage mixing: putting natural rubber STR20 and styrene butadiene rubber SBR1502 into an internal mixer, dropping an upper top bolt, opening the upper top bolt after 40 seconds, adding zinc oxide, stearic acid, an anti-aging agent 4020 and microcrystalline wax, and dropping the upper top bolt; after 30 seconds, opening the upper top bolt, adding 1/2 white carbon black, and dropping the upper top bolt; after 30 seconds, opening the upper top bolt, adding V700, the light-colored solid silane coupling agent and the residual white carbon black, dropping the upper top bolt, lifting the bolt every other minute to clean leaked rubber, mixing for 7 minutes, discharging a section of master rubber at the rubber discharge temperature of 145 ℃, and discharging and cooling the section of master rubber through a mill for discharging;
and (3) second-stage mixing: putting the first-stage masterbatch into the internal mixer again for two-stage mixing for 5 minutes, lifting the plug every other minute to clean leaked rubber, discharging the second-stage masterbatch when the rubber discharge temperature is 145 ℃, and discharging the second-stage masterbatch through an open mill for sheet discharging and cooling;
and (3) final refining: thinning the second-stage masterbatch again through an open mill, wrapping the rubber material with a roller, adding an accelerator DPG, an accelerator CZ and sulfur, cutting twice with a left cutter and a right cutter, and after feeding, alternately performing rolling and triangular wrapping for four times respectively and discharging;
and (3) vulcanization: the vulcanization characteristic of the rubber material is measured by a rotor-free vulcanizer, the vulcanization temperature is set to be 150 ℃, the vulcanization pressure is set to be 11MPa, and the vulcanization time is set to be 1.3 Xt 90.
Example 2:
this example relates to performance testing of composites prepared with the light-colored solid silane coupling agent of example 1, replacing the light-colored solid silane coupling agent of example 1 with a silane coupling agent having a mass ratio of 1: the carbon black of 1 is mixed with liquid Si69, and the carbon black silane coupling agent prepared by uniformly stirring is the formula of comparative example 1, and the formula of the composite material prepared by the comparative example 1 comprises the following components in parts by weight: 2025 parts of natural rubber STR, 150275 parts of styrene butadiene rubber SBR, 75 parts of white carbon black, 20 parts of carbon black silane coupling agent, V70025 parts, 2 parts of stearic acid, 2 parts of zinc oxide, 40202 parts of anti-aging agent, 1.5 parts of microcrystalline wax, 1.2 parts of accelerator DPG, 2.5 parts of accelerator CZ and 1.25 parts of sulfur; a composite material was prepared according to the specific procedure for preparing a composite material of example 1;
the composites prepared in example 1 and comparative example 1 were tested separately and the results are shown in the following table:
| test items | Comparative example 1 | Example 1 |
| Mooney viscosity/MU | 45.62 | 42.37 |
| T10/min | 1.58 | 5.68 |
| T90/min | 27.71 | 30.28 |
| 10% stress at definite elongation/MPa | 1.11 | 1.11 |
| 50% stress at definite elongation/MPa | 1.78 | 1.98 |
| 100% stress at definite elongation/MPa | 2.57 | 3.16 |
| 200% stress at definite elongation/MPa | 5.25 | 6.66 |
| 300% stress at definite elongation/MPa | 8.40 | 10.43 |
| Elongation at break/% | 528.82 | 559.38 |
| Tensile strength/MPa | 15.33 | 19.93 |
| Tensile product coefficient | 8105.72 | 11150.89 |
| Tear Strength/K.mm-1 | 56.09 | 58.65 |
| Rebound Rate/%) | 37.55 | 37.70 |
| DIN abrasion/mm3 | 151 | 143 |
| ΔG'/kPa | 392 | 379 |
| tanδ@0℃ | 0.20 | 0.21 |
| tanδ@60℃ | 0.13 | 0.12 |
Wherein: t10 is the initial vulcanization time, and is related to the scorching time of the rubber compound, and the longer T10 is, the longer the scorching time is, the higher the processing safety of the rubber compound is; the tan delta @0 ℃ is a loss factor of the rubber material at 0 ℃, the tan delta @0 ℃ can predict the wet skid resistance of the rubber material when the rubber material is used for a tire tread, and the larger the tan delta @0 ℃, the better the wet skid resistance; the tan delta @60 ℃ is a loss factor of the rubber compound at 60 ℃, the tan delta @60 ℃ can predict the rolling resistance of the rubber compound when the rubber compound is used for a tire tread, and the lower the tan delta @60 ℃, the smaller the rolling resistance.
As can be seen from the table: the Mooney viscosity of example 1 was reduced compared to that of comparative example 1; t10 of example 1 is significantly greater than that of comparative example 1, indicating that the light-colored solid silane coupling agent N can effectively improve the processing safety of the sizing material; the stress at definite elongation, the tensile strength, the elongation at break, the tensile product coefficient and the tear strength of the composite material in example 1 are all improved compared with those of the composite material in comparative example 1, the tensile strength is improved by 30.0%, and the tensile product coefficient is improved by 37.6%, which shows that the light-colored solid silane coupling agent can improve the physical and mechanical properties of the composite material; the rebound resilience of example 1 is kept at the same level as that of comparative example 1; the abrasion and Δ G' of example 1 was slightly less than that of comparative example 1; the tan delta @0 ℃ of example 1 is greater than the tan delta @0 ℃ of comparative example 1, indicating that the wet skid resistance of example 1 is better; the tan delta @60 ℃ of example 1 is smaller than the tan delta @60 ℃ of comparative example 1, indicating that the rolling resistance is smaller when example 1 is used for a tire tread, and the energy loss, dynamic hysteresis, and heat generation generated during a stress can be reduced.
Example 3:
the light-colored solid silane coupling agent related to the embodiment is prepared from 2 parts by weight of a silane coupling agent, wherein the whiteness is 85, the median particle diameter D50 is 3.08 mu m, and the length-diameter ratio is 10: 1 wollastonite and 1 part by mass of liquid Si69, and stirring the mixture evenly to prepare the silicon dioxide coating,
the formula for preparing the composite material by using the light-colored solid silane coupling agent comprises the following components in parts by weight: natural rubber STR20100 parts, white carbon black 60 parts, light-color solid silane coupling agent 15 parts, stearic acid 2 parts, zinc oxide 2 parts, anti-aging agent 40202 parts, accelerator DPG 1.3 parts, accelerator CZ 1.2 parts and sulfur 1 part; the specific process for preparing the composite material comprises the following steps:
first-stage mixing: the natural rubber STR20 is subjected to thin pass plastication for 2 times through an open mill and then is put into an internal mixer, an upper top bolt falls down, after 40 seconds, the upper top bolt is opened, and zinc oxide, stearic acid and an anti-aging agent 4020 are added to fall down the upper top bolt; after 30 seconds, opening the upper top bolt, adding 1/2 white carbon black, and dropping the upper top bolt; after 30 seconds, opening the upper top plug, adding the light-colored solid silane coupling agent and the residual 1/2 white carbon black, dropping the upper top plug, lifting the plug every other minute to clean leaked rubber, mixing for 7 minutes, discharging a section of master rubber at the rubber discharge temperature of 145 ℃, and discharging and cooling the section of master rubber through a mill for discharging;
and (3) second-stage mixing: putting the first-stage masterbatch into the internal mixer again for two-stage mixing for 5 minutes, lifting the plug every other minute to clean leaked rubber, discharging the second-stage masterbatch when the rubber discharge temperature is 145 ℃, and discharging the second-stage masterbatch through an open mill for sheet discharging and cooling;
and (3) final refining: thinning the second-stage masterbatch again through an open mill, wrapping the rubber material with a roller, adding an accelerator DPG, an accelerator CZ and sulfur, cutting twice with a left cutter and a right cutter, and after feeding, alternately performing rolling and triangular wrapping for four times respectively and discharging;
and (3) vulcanization: the vulcanization characteristic of the rubber material is measured by a rotor-free vulcanizer, the vulcanization temperature is set to be 150 ℃, the vulcanization pressure is set to be 11MPa, and the vulcanization time is set to be 1.3 Xt 90.
Example 4:
this example relates to performance testing of composites prepared with the light-colored solid silane coupling agent of example 3, replacing the light-colored solid silane coupling agent of example 3 with a silane coupling agent having a mass ratio of 1: 1 and liquid Si69, and the carbon black silane coupling agent prepared by uniformly stirring is the formula of comparative example 2, and the formula for preparing the composite material of comparative example 2 comprises the following components in parts by weight: 2025 parts of natural rubber STR, 150275 parts of styrene butadiene rubber SBR, 75 parts of white carbon black, 20 parts of carbon black silane coupling agent, V70025 parts, 2 parts of stearic acid, 2 parts of zinc oxide, 40202 parts of anti-aging agent, 1.5 parts of microcrystalline wax, 1.2 parts of accelerator DPG, 2.5 parts of accelerator CZ and 1.25 parts of sulfur; a composite material was prepared according to the specific procedure for preparing a composite material of example 3;
the composites prepared in example 3 and comparative example 2 were tested separately and the results are shown in the following table:
| test items | Comparative example 2 | Example 3 |
| Mooney viscosity/MU | 43.16 | 39.53 |
| T10/min | 1.67 | 3.13 |
| T90/min | 14 | 15.38 |
| 10% stress at definite elongation/MPa | 0.93 | 1.11 |
| 50% stress at definite elongation/MPa | 1.67 | 1.80 |
| 100% stress at definite elongation/MPa | 2.66 | 2.75 |
| 200% stress at definite elongation/MPa | 6.29 | 6.65 |
| 300% stress at definite elongation/MPa | 11.35 | 12.04 |
| Elongation at break/% | 577.73 | 589.90 |
| Tensile strength/MPa | 26.68 | 26.94 |
| Tensile product | 15413.84 | 15891.91 |
| Tear Strength/K.mm-1 | 134.81 | 137.77 |
| Rebound Rate/%) | 50.4 | 54.0 |
| DIN abrasion/mm3 | 164 | 160 |
| ΔG'/kPa | 301.28 | 243.33 |
As can be seen from the table: the Mooney viscosity of example 3 was reduced by nearly 4 units compared to the Mooney viscosity of comparative example 2; t10 of example 3 is significantly greater than that of comparative example 2, indicating that the light-colored solid silane coupling agent can effectively improve the processing safety of the compound; the stress at definite elongation, tensile strength, elongation at break, product coefficient of tensile strength and tear strength of example 3 are all improved as compared to those of comparative example 2; the rebound resilience of the example 3 is improved by 7.2 percent compared with the rebound resilience of the comparative example 2; the DIN abrasion of example 3 was at the same performance level as the DIN abrasion of comparative example 2; Δ G 'for example 3 is less than Δ G' for comparative example 2, indicating that the filler dispersion is better in example 3.
Claims (9)
1. A light-colored solid silane coupling agent is characterized by comprising wollastonite and a silane coupling agent.
2. The light-colored solid silane coupling agent of claim 1, wherein the wollastonite is present in an amount of 10 parts by weight and the silane coupling agent is present in an amount of 1 to 10 parts by weight.
3. A light-colored solid silane coupling agent according to claim 1 or 2, wherein the wollastonite has a structure including needle-like, fiber-like and strand-like structures.
4. A light-colored solid silane coupling agent according to claim 3, wherein the whiteness of the wollastonite is 50 to 90.
5. A light-colored solid silane coupling agent according to claim 1 or 2, wherein the silane coupling agent is in a liquid state.
6. The light-colored solid silane coupling agent of claim 5, wherein the silane coupling agent comprises Si69, Si75, and KH-550.
7. A light-colored solid silane coupling agent according to claim 1 or 2, which is capable of replacing a conventional solid silane coupling agent comprising carbon black as a carrier in an equivalent amount to prepare a rubber article.
8. The silane coupling agent of claim 3, wherein the wollastonite has a median particle diameter D50 of 1 to 20 μm.
9. The light-colored solid silane coupling agent of claim 8, wherein the wollastonite has an aspect ratio of 1 to 20: 1.
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