CN113583460A - Bio-based modified low-heat-generation reinforcing agent and preparation method thereof - Google Patents
Bio-based modified low-heat-generation reinforcing agent and preparation method thereof Download PDFInfo
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- CN113583460A CN113583460A CN202110683119.3A CN202110683119A CN113583460A CN 113583460 A CN113583460 A CN 113583460A CN 202110683119 A CN202110683119 A CN 202110683119A CN 113583460 A CN113583460 A CN 113583460A
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- 239000012744 reinforcing agent Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 79
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000003208 petroleum Substances 0.000 claims abstract description 25
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 22
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 19
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 16
- 239000005011 phenolic resin Substances 0.000 claims abstract description 16
- 239000011787 zinc oxide Substances 0.000 claims abstract description 16
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- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 13
- 239000011707 mineral Substances 0.000 claims abstract description 13
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 12
- 229920005551 calcium lignosulfonate Polymers 0.000 claims abstract description 12
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims abstract description 12
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920005552 sodium lignosulfonate Polymers 0.000 claims abstract description 12
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- 238000000034 method Methods 0.000 claims abstract description 10
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 10
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008117 stearic acid Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 230000020169 heat generation Effects 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 91
- 238000000227 grinding Methods 0.000 claims description 20
- 230000004048 modification Effects 0.000 claims description 17
- 238000012986 modification Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 230000008878 coupling Effects 0.000 claims description 7
- 238000010168 coupling process Methods 0.000 claims description 7
- 238000005859 coupling reaction Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229910052900 illite Inorganic materials 0.000 claims description 6
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 6
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 claims description 6
- 239000005995 Aluminium silicate Substances 0.000 claims description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000000440 bentonite Substances 0.000 claims description 4
- 229910000278 bentonite Inorganic materials 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000003623 enhancer Substances 0.000 claims 1
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- 229920001971 elastomer Polymers 0.000 abstract description 28
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- 230000000694 effects Effects 0.000 abstract description 26
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- 239000010959 steel Substances 0.000 abstract description 2
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- 238000004513 sizing Methods 0.000 description 5
- 238000004537 pulping Methods 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000003139 buffering effect Effects 0.000 description 2
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- 239000006185 dispersion Substances 0.000 description 2
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- 244000043261 Hevea brasiliensis Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
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- 239000000945 filler Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention relates to a low-heat-generation reinforcing agent modified by a bio-base, which comprises the following raw materials: the coating comprises a non-metal mineral material, 10% by mass of sodium chloride, 20% by mass of calcium carbonate solution, calcium lignosulfonate, sodium lignosulfonate, alkali lignin, coumarone, petroleum resin C5, petroleum resin C9, urotropine, stearic acid, zinc oxide, a silane coupling agent Si-69 and phenolic resin. The invention also provides a preparation method of the low-heat-generation reinforcing agent modified by the bio-based method. The reinforcing agent has high surface activity, is easy to mix into rubber material, has good processing technology, can effectively reduce the compression heat generation of the rubber material, improves the bonding effect of the tire body and the cord fabric rubber material with the belted layer and the steel wire, improves the physical and mechanical properties of the rubber material such as aging resistance and the like, and can partially replace carbon black and white carbon black.
Description
Technical Field
The invention relates to the technical field of rubber reinforcing fillers, in particular to a low-heat-generation reinforcing agent modified by a bio-base and a preparation method thereof.
Background
At present, the reinforcing agent for rubber is mainly carbon black, white carbon black, lignin and a low-heat-generation reinforcing agent modified by a bio-based, and is prepared by compounding and mixing lignin, a bio-based modified material, a functional organic material and a modified kaolin, illite and other non-metal mineral nano materials. Can replace about 30 percent of carbon black and white carbon black, reduces the consumption of the carbon black and saves petroleum energy used for producing the carbon black. The reinforcing agent is used in a sizing material together with carbon black and white carbon black to play a synergistic effect, and when the reinforcing agent is used in a tire sizing material, the performance of the sizing material can not only keep the original characteristics, but also obviously reduce the heat buildup property of the tire, and prolong the service life of the tire. The reinforcing agent has the effects of enhancing rubber, bonding, aging resistance and the like. The material can relatively reduce the dosage of adhesive and anti-aging agent in the rubber formula, and has good cost performance advantage. Thereby filling the blank of applying the lignin in the tires in the domestic rubber industry.
The existing modified products of non-metallic mineral materials such as kaolin, illite and the like are generally modified by adding a certain amount of silane coupling agent or titanate and aluminate coupling agent into a 4000-mesh product, adding glacial acetic acid and ethanol, and completing the modification of the product through dry kneading or wet aging and precipitation. The modification method has the defects of high production cost and low quality, particularly, when the produced product is used for production in the rubber field, powder eating is difficult, the quality of rubber products is low, when the product is used for natural rubber and various synthetic rubbers, the product is not as good as common fillers such as calcium carbonate, pottery clay and the like in reinforcing property, the comprehensive performance of rubber materials is not ideal, certain influence is caused on vulcanization, and the performance of the product is influenced by a large amount of filling, so that the product cannot be widely used for various rubber products.
The other important factor of the problems is that when the materials are mixed, the contact area between the materials is reduced due to the defects of mixing equipment, so that high-quality mixing cannot be realized, and the modification effect of the non-metallic mineral material is influenced.
Disclosure of Invention
The invention aims to provide a low-heat-generation reinforcing agent modified by a bio-base and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a low-heat-generation reinforcing agent modified by a bio-based material comprises the following raw materials in parts by weight: 80-120 parts of non-metallic mineral material, 2-5 parts of sodium chloride with the mass fraction of 10%, 3-6 parts of calcium carbonate solution with the mass fraction of 20%, 10-20 parts of calcium lignosulfonate, 15-25 parts of sodium lignosulfonate, 8-16 parts of alkali lignin, 8-16 parts of coumarone, 8-8 parts of petroleum resin C54, C93-9 parts of petroleum resin, 2-8 parts of urotropine, 1-5 parts of stearic acid, 4-9 parts of zinc oxide, 4-693-9 parts of silane coupling agent and 4-8 parts of phenolic resin.
Preferably, the non-metallic mineral material is one or a mixture of more than two of kaolin, illite, bentonite, silicon micropowder and talcum powder.
The invention also provides a preparation method of the low-heat-generation reinforcing agent modified by the bio-base, which comprises the following steps:
s1, smashing, desanding and grinding a non-metallic mineral material to a particle size of 5-15 microns, adding 10% by mass of sodium chloride and 20% by mass of calcium carbonate solution, stirring at a rotation speed of 850r/min for 20-40min at 650-;
s2, adding the modification auxiliary agent, zinc oxide, calcium lignosulfonate, sodium lignosulfonate, alkali lignin, petroleum resin C5, petroleum resin C5, phenolic resin, urotropine and silane coupling agent KH-550 into a stirring kettle, stirring and mixing, heating to 95-105 ℃, stirring at the rotating speed of 650 plus 850r/min for 1-2h, and cooling to room temperature to obtain the low-heat-generation reinforcing agent modified by the bio-based.
Preferably, the stirred tank includes the cauldron body and locates the internal cauldron chamber of the internal cauldron of cauldron, the upper end of the cauldron body is equipped with first inlet pipe and second inlet pipe, the lower extreme of the cauldron body is equipped with the discharging pipe, the upper end of the cauldron body is equipped with the motor, the lower extreme of motor is equipped with the shaft coupling, the one end that the motor was kept away from to the shaft coupling is equipped with the pivot, the pivot is equipped with the rotor plate in the cauldron intracavity, one side that the rotor plate is close to the internal wall of cauldron is equipped with first mounting panel, one side that first mounting panel is close to the internal wall of cauldron is equipped with the second mounting panel, one side that the second mounting panel is close to the internal wall of cauldron is equipped with the first arch of grinding of a plurality of.
Preferably, a plurality of first springs are arranged between the first mounting plate and the second mounting plate.
Preferably, the lower extreme of pivot is installed along the stirring board that the pivot centrosymmetric set up, one side that the stirring board is close to the internal wall of cauldron is equipped with a plurality of second and grinds the arch.
Preferably, be equipped with first hinge in the pivot, be equipped with first piston on the first hinge, one side that first piston is close to the stirring board is equipped with first piston, one side that first piston is close to the stirring board is equipped with the piston axle, one side that the piston axle is close to the stirring board is equipped with the second piston, be equipped with the second hinge on the stirring board, the second piston is rotatory to be installed on the second hinge, be equipped with the second spring between first piston and the second piston, the second spring cup joints the periphery at the piston axle.
Preferably, the gap between the second grinding bulge and the inner wall of the kettle body is m, and m is more than 0 and less than or equal to 2 cm.
Preferably, the included angle between the stirring plate and the vertical direction is alpha, and alpha is more than or equal to 30 degrees and less than or equal to 80 degrees.
Preferably, the periphery of pivot is equipped with the stirring leaf, be equipped with a plurality of reposition of redundant personnel hole on the stirring leaf, the periphery of pivot still is equipped with the guide shaft cover, be equipped with the mounting disc that is located the cauldron intracavity on the guide shaft cover, be equipped with the through-hole in the mounting disc.
Compared with the prior art, the invention has the beneficial effects that:
1. kaolin, illite, bentonite, silicon micropowder and talcum powder are modified by a silane coupling agent Si-69, then are mixed with stearic acid, zinc oxide and phenolic resin to obtain a modification aid, and zinc oxide, calcium lignosulfonate, sodium lignosulfonate, alkali lignin, petroleum resin C5, petroleum resin C5, phenolic resin and urotropine are added again, and a silane coupling agent KH-550 is used as a modifier for grafting modification again, so that two times of grafting modification are realized, so that the silane coupling agent S i-69 and the silane coupling agent KH-550 can be used for grafting modification for multiple times, a better grafting connection effect can be formed between a bio-based raw material and rubber after modification, the rubber reinforcing effect is improved, the reinforcing agent has high surface activity, rubber sizing materials are easy to mix, and the processing process is good, the compression heat generation of the rubber material can be effectively reduced, the bonding effect of the rubber material of the tire body and the cord fabric with the belted layer and the steel wire is improved, the physical and mechanical properties of the rubber material such as aging resistance and the like are improved, and the rubber material can partially replace carbon black and white carbon black.
2. The rubber is suitable for rubbers with different viscosities or different polarities (NR, BR, SBR, EPDM, etc.), and can also be used in a single rubber. Can be used in non-tire rubber products such as tires, conveying belts, rubber tubes, gaskets, shoe materials, automobile sealing parts and the like.
3. By the rotation of motor drive pivot, rotatory by pivot rotation drive rotor plate, the rotatory first material of grinding arch to attaching to on the internal wall of cauldron of realizing of rotor plate grinds, realizes further stirring grinding when the material stirring mixes, so can effectively improve the efficiency and the quality that the material mixes, has increased area of contact between the material, so can improve comprehensive properties such as reinforcing of reinforcing agent to rubber sizing material.
4. Through establishing the first spring of a plurality of between first mounting panel and second mounting panel, the setting of first spring can provide the holding power for the stirring board, so effectively improved the efficiency and the quality that the material mixes the stirring, and then improved the homogeneity effect that the material is modified.
5. Install the stirring board that sets up along pivot central symmetry through the lower extreme in the pivot to it grinds the arch to establish a plurality of second near cauldron internal wall one side at the stirring board, so can realize the grinding to the material, has improved the efficiency and the quality that the material stirring mixes, and then has improved the homogeneity effect that the material was modified.
6. The piston shaft stretches out and draws back between first piston and second piston, has realized that the stirring board has certain activity space, so can improve the efficiency and the quality that the material mixes the stirring, and then improved the homogeneity effect that the material was modified.
7. The setting of second spring can realize the buffering shock attenuation, so effectively improve the stability of stirring board stirring, avoid the second to grind protruding jam, effectively improve the efficiency and the quality that the material stirring was mixed, and then improved the homogeneity effect that the material was modified.
8. Specifically to in this embodiment, m is 1cm, so set up and to avoid the material to block up, improves the efficiency and the quality that the material stirring was mixed, and then has improved the homogeneity effect that the material was modified.
9. Particularly in this embodiment, alpha is 55 degrees, so set up the quality that can effectively improve the material stirring and mix, and then improved the homogeneity effect of material modification.
10. Establish the stirring leaf through the periphery at the pivot, be equipped with a plurality of diffluence holes on the stirring leaf, the effect that the material dispersion can be improved in the setting of diffluence hole, improves the quality that the material stirring was mixed, and then has improved the modified homogeneity effect of material, and in addition, the direction axle sleeve relies on the mounting disc can effectively improve the rotatory stability of pivot.
Drawings
FIG. 1 is a schematic structural diagram of a first stirring kettle and a second stirring kettle in the preparation method of the bio-based modified low-heat-generation reinforcing agent;
FIG. 2 is an enlarged view of a portion of FIG. 1 at A;
fig. 3 is a partially enlarged schematic view of a portion B in fig. 2.
In the figure: 1. a kettle body; 2. a kettle cavity; 3. a discharge pipe; 4. a motor; 5. a rotating shaft; 6. a coupling; 7. A first feed tube; 8. a second feed tube; 9. stirring blades; 10. a shunt hole; 11. a guide shaft sleeve; 12. A through hole; 13. mounting a disc; 14. a rotating plate; 15. a first mounting plate; 16. a first spring; 17. a second mounting plate; 18. a first grinding projection; 19. a first hinge; 20. a first piston; 21. a piston shaft; 22. a second piston; 23. a second spring; 24. a second hinge; 25. a stirring plate; 26. and a second grinding bump.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A low-heat-generation reinforcing agent modified by a bio-based material comprises the following raw materials in parts by weight: 100 parts of kaolin, 2-5 parts of sodium chloride with the mass fraction of 10%, 3-6 parts of calcium carbonate solution with the mass fraction of 20%, 10-20 parts of calcium lignosulfonate, 15-25 parts of sodium lignosulfonate, 8-16 parts of alkali lignin, 8-16 parts of coumarone, 8-8 parts of petroleum resin C54, C93-9 parts of petroleum resin, 2-8 parts of urotropine, 1-5 parts of stearic acid, 4-9 parts of zinc oxide, 4-693-9 parts of silane coupling agent and 4-8 parts of phenolic resin.
The invention also provides a preparation method of the low-heat-generation reinforcing agent modified by the bio-base, which comprises the following steps:
s1, pulping, desanding and grinding a non-metallic mineral material to a particle size of 10 microns, adding 10% by mass of sodium chloride and 20% by mass of a calcium carbonate solution, stirring at a rotating speed of 750r/min for 30min, heating to 85 ℃, keeping for 13min, stirring at a rotating speed of 2000r/min for 55min, adding a silane coupling agent Si-69 and stearic acid, mixing, keeping for 10min, continuously stirring at a high speed, heating to 100 ℃, adding zinc oxide and phenolic resin, and keeping for 10min to obtain a modification aid;
s2, adding the modification auxiliary agent, zinc oxide, calcium lignosulfonate, sodium lignosulfonate, alkali lignin, petroleum resin C5, petroleum resin C5, phenolic resin, urotropine and a silane coupling agent KH-550 into a stirring kettle, stirring and mixing, heating to 100 ℃, stirring at a rotating speed of 750r/min for 1.5h, and cooling to room temperature to obtain the low-heat-generation reinforcing agent modified by the bio-based.
As shown in fig. 1-2, stirred tank includes the cauldron body 1 and locates the cauldron cavity 2 of the internal 1 internal cauldron of cauldron body 1, the upper end of the cauldron body 1 is equipped with first inlet pipe 7 and second inlet pipe 8, the lower extreme of the cauldron body 1 is equipped with discharging pipe 3, the upper end of the cauldron body 1 is equipped with motor 4, the lower extreme of motor 4 is equipped with shaft coupling 6, the one end that motor 4 was kept away from to the shaft coupling is equipped with pivot 5, pivot 5 is equipped with rotor plate 14 in cauldron cavity 2, one side that rotor plate 14 is close to the internal wall of cauldron 1 is equipped with first mounting panel 15, one side that first mounting panel 15 is close to the internal wall of cauldron 1 is equipped with second mounting panel 17, one side that second mounting panel 17 is close to the internal wall of cauldron 1 is equipped with the first arch 18 of a plurality of grinding. By the 5 rotations of motor 4 drive pivot, rotatory drive rotor plate 14 is rotatory by pivot 5, and rotor plate 14 is rotatory to be realized first protruding 18 of grinding and to grind the material of attaching to on the 1 inner wall of the cauldron body, realizes further stirring grinding when the material stirring mixes, so can effectively improve the efficiency and the quality that the material mixes, has increased the area of contact between the material, so can strengthen the effect of reinforcing agent in the rubber reinforcement.
In the present embodiment, a plurality of first springs 16 are disposed between the first mounting plate 15 and the second mounting plate 17. Through establishing the first spring 16 of a plurality of between first mounting panel 15 and second mounting panel 17, the setting of first spring 16 can provide the holding power for stirring board 25, so effectively improved the efficiency and the quality that the material mixes the stirring, and then improved the homogeneity effect that the material is modified.
In this embodiment, the lower extreme of pivot 5 is installed and is followed 5 centrosymmetric stirring boards 25 that set up of pivot, one side that stirring board 25 is close to the internal wall of cauldron 1 is equipped with a plurality of second and grinds arch 26. Install the stirring board 25 that sets up along 5 centrosymmetries of pivot through the lower extreme at pivot 5 to establish a plurality of second and grind protruding 26 near cauldron body 1 inner wall one side at stirring board 25, so can realize the grinding to the material, improved the efficiency and the quality that the material stirring was mixed, and then improved the homogeneity effect that the material was modified.
In this embodiment, be equipped with first hinge 19 on pivot 5, be equipped with first piston 20 on first hinge 19, one side that first piston 20 is close to stirring board 25 is equipped with first piston 20, one side that first piston 20 is close to stirring board 25 is equipped with piston shaft 21, one side that piston shaft 21 is close to stirring board 25 is equipped with second piston 22, be equipped with second hinge 24 on the stirring board 25, second piston 22 is rotatory to be installed on second hinge 24. Piston shaft 21 is flexible between first piston 20 and second piston 22, has realized that stirring board 25 has certain activity space, so can improve the efficiency and the quality that the material mixes the stirring, and then improved the homogeneity effect that the material is modified.
In the present embodiment, a second spring 23 is disposed between the first piston 20 and the second piston 22, and the second spring 23 is sleeved on the outer periphery of the piston shaft 21. Buffering shock attenuation can be realized in the setting of second spring 23, so effectively improve the stability of stirring board 25, avoid the second to grind protruding 26 and block up, effectively improve the efficiency and the quality that the material stirring mixes, and then improved the modified homogeneity effect of material.
In this embodiment, the gap between the second grinding protrusion 26 and the inner wall of the kettle 1 is m, where m is greater than 0 and less than or equal to 2 cm. Specifically to in this embodiment, m is 1cm, so set up and to avoid the material to block up, improves the efficiency and the quality that the material stirring was mixed, and then has improved the homogeneity effect that the material was modified.
In the embodiment, the included angle between the stirring plate 25 and the vertical direction is alpha, and alpha is more than or equal to 30 degrees and less than or equal to 80 degrees. Particularly in this embodiment, alpha is 55 degrees, so set up the quality that can effectively improve the material stirring and mix, and then improved the homogeneity effect of material modification.
In this embodiment, the periphery of pivot 5 is equipped with stirring leaf 9, be equipped with a plurality of reposition of redundant personnel hole on the stirring leaf 9, the periphery of pivot 5 still is equipped with guide shaft sleeve 11, be equipped with the mounting disc 13 that is located cauldron cavity 2 on the guide shaft sleeve 11, be equipped with through-hole 12 in the mounting disc 13. Establish stirring leaf 9 through the periphery at pivot 5, establish a plurality of diffluence holes 10 on the stirring leaf 9, the effect that the material dispersion can be improved in the setting of diffluence hole 10, improves the quality that the material stirring was mixed, and then has improved the homogeneity effect that the material was modified, in addition, the guide shaft cover 11 relies on in mounting disc 13 can effectively improve the rotatory stability of pivot 5.
It will be appreciated that m may also be 1mm, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 11mm, 12mm, 13mm, 14mm, 15mm, 16mm, 17mm, 18mm, 19mm, 20mm etc.
It is to be understood that α can also be 30 °, 31 °, 32 °, 33 °, 34 °, 35 °, 36 °, 37 °, 38 °, 39 °, 40 °, 41 °, 42 °, 43 °, 44 °, 45 °, 46 °, 47 °, 48 °, 49 °, 50 °, 51 °, 52 °, 53 °, 54 °, 56 °, 57 °, 58 °, 59 °, 60 °, 61 °, 62 °, 63 °, 64 °, 65 °, 66 °, 67 °, 68 °, 69 °, 70 °, 71 °, 72 °, 73 °, 74 °, 75 °, 76 °, 77 °, 78 °, 79 °, 80 °, etc.
Example 2
A low-heat-generation reinforcing agent modified by a bio-based material comprises the following raw materials in parts by weight: 80 parts of illite, 5 parts of sodium chloride with the mass fraction of 10%, 3 parts of calcium carbonate solution with the mass fraction of 20%, 20 parts of calcium lignosulfonate, 15 parts of sodium lignosulfonate, 16 parts of alkali lignin, 8 parts of coumarone, C58 parts of petroleum resin, C93 parts of petroleum resin, 8 parts of urotropine, 1 part of stearic acid, 9 parts of zinc oxide, Si-693 parts of a silane coupling agent and 8 parts of phenolic resin.
The invention also provides a preparation method of the low-heat-generation reinforcing agent modified by the bio-base, which comprises the following steps:
s1, pulping, desanding and grinding a non-metallic mineral material to a particle size of 5 microns, adding 10% by mass of sodium chloride and 20% by mass of a calcium carbonate solution, stirring at a rotating speed of 850r/min for 20min, heating to 90 ℃ and keeping for 10min, stirring at a rotating speed of 2500r/min for 50min, adding a silane coupling agent Si-69 and stearic acid, mixing, keeping for 15min, continuously stirring at a high speed, heating to 95 ℃, adding zinc oxide and phenolic resin, and keeping for 15min to obtain a modification aid;
s2, adding the modification auxiliary agent, zinc oxide, calcium lignosulfonate, sodium lignosulfonate, alkali lignin, petroleum resin C5, petroleum resin C5, phenolic resin, urotropine and a silane coupling agent KH-550 into a stirring kettle, stirring and mixing, heating to 95 ℃, stirring at the rotating speed of 850r/min for 1h, and cooling to room temperature to obtain the low-heat-generation reinforcing agent modified by the bio-base.
Example 3
A low-heat-generation reinforcing agent modified by a bio-based material comprises the following raw materials in parts by weight: 120 parts of bentonite, 2 parts of sodium chloride with the mass fraction of 10%, 6 parts of calcium carbonate solution with the mass fraction of 20%, 10 parts of calcium lignosulfonate, 25 parts of sodium lignosulfonate, 8 parts of alkali lignin, 16 parts of coumarone, C54 parts of petroleum resin, C99 parts of petroleum resin, 2 parts of urotropine, 5 parts of stearic acid, 4 parts of zinc oxide, Si-699 parts of a silane coupling agent and 4 parts of phenolic resin.
The invention also provides a preparation method of the low-heat-generation reinforcing agent modified by the bio-base, which comprises the following steps:
s1, pulping, desanding and grinding a non-metallic mineral material to a particle size of 15 microns, adding 10% by mass of sodium chloride and 20% by mass of a calcium carbonate solution, stirring at a rotating speed of 650r/min for 40min, heating to 80 ℃ and keeping for 15min, stirring at a rotating speed of 1500r/min for 60min, adding a silane coupling agent Si-69 and stearic acid, mixing, keeping for 5min, continuing to stir at a high speed and heating to 105 ℃, adding zinc oxide and phenolic resin, and keeping for 5min to obtain a modification aid;
s2, adding the modification auxiliary agent, zinc oxide, calcium lignosulfonate, sodium lignosulfonate, alkali lignin, petroleum resin C5, petroleum resin C5, phenolic resin, urotropine and a silane coupling agent KH-550 into a stirring kettle, stirring and mixing, heating to 105 ℃, stirring at the rotating speed of 650r/min for 2h, and cooling to room temperature to obtain the low-heat-generation reinforcing agent modified by the bio-base.
The performance of the test formulation using the reinforcing agent of the present invention in combination with carbon black was compared with the normal formulation and the data obtained are shown in tables 1 to 4 below:
TABLE 1 vulcanization characteristics of the compounds
TABLE 2 physical Properties of the rubber compositions
*: the compression heat generation is 151 ℃ multiplied by 30', the prestress is 1.0MPa, and the stroke is 4.45 nm.
TABLE 3 compression Heat buildup test (variants of the invention)
*: the compression heat generation is 151 ℃ multiplied by 30', the prestress is 1.0MPa, and the stroke is 4.45 nm.
TABLE 4 indoor durability test data (12R22.518PR)
Note: the test speed of the indoor durability test is 65 km/h.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A low-heat-generation reinforcing agent modified by a bio-based material is characterized by comprising the following raw materials in parts by weight: 80-120 parts of non-metallic mineral material, 2-5 parts of sodium chloride with the mass fraction of 10%, 3-6 parts of calcium carbonate solution with the mass fraction of 20%, 10-20 parts of calcium lignosulfonate, 15-25 parts of sodium lignosulfonate, 8-16 parts of alkali lignin, 8-16 parts of coumarone, 8-8 parts of petroleum resin C54, C93-9 parts of petroleum resin, 2-8 parts of urotropine, 1-5 parts of stearic acid, 4-9 parts of zinc oxide, 4-693-9 parts of silane coupling agent and 4-8 parts of phenolic resin.
2. The method for preparing the bio-based modified low-heat-generation reinforcing agent according to claim 1, wherein the non-metallic mineral material is one or a mixture of more than two of kaolin, illite, bentonite, silica micropowder and talcum powder.
3. A method for preparing a bio-based modified low-heat-buildup reinforcing agent according to claim 1 or 2, comprising the steps of:
s1, smashing, desanding and grinding a non-metallic mineral material to a particle size of 5-15 microns, adding 10% by mass of sodium chloride and 20% by mass of calcium carbonate solution, stirring at a rotation speed of 850r/min for 20-40min at 650-;
s2, adding the modification auxiliary agent, zinc oxide, calcium lignosulfonate, sodium lignosulfonate, alkali lignin, petroleum resin C5, petroleum resin C5, phenolic resin, urotropine and silane coupling agent KH-550 into a stirring kettle, stirring and mixing, heating to 95-105 ℃, stirring at the rotating speed of 650 plus 850r/min for 1-2h, and cooling to room temperature to obtain the low-heat-generation reinforcing agent modified by the bio-based.
4. The preparation method of the low-heat-generation reinforcing agent modified by the bio-based material as claimed in claim 3, wherein the stirring kettle comprises a kettle body and a kettle cavity arranged in the kettle body, the upper end of the kettle body is provided with a first feeding pipe and a second feeding pipe, the lower end of the kettle body is provided with a discharging pipe, the upper end of the kettle body is provided with a motor, the lower end of the motor is provided with a shaft coupling, one end of the shaft coupling, which is far away from the motor, is provided with a rotating shaft, the rotating shaft is provided with a rotating plate in the kettle cavity, one side of the rotating plate, which is close to the inner wall of the kettle body, is provided with a first mounting plate, one side of the first mounting plate, which is close to the inner wall of the kettle body, is provided with a second mounting plate, and one side of the second mounting plate, which is close to the inner wall of the kettle body, is provided with a plurality of first grinding protrusions.
5. The method for preparing the bio-based modified low heat generation enhancer as claimed in claim 4, wherein a plurality of first springs are disposed between the first mounting plate and the second mounting plate.
6. The method for preparing the bio-based modified low-heat-generation reinforcing agent according to claim 4, wherein the lower end of the rotating shaft is provided with a stirring plate which is arranged along the center of the rotating shaft symmetrically, and one side of the stirring plate close to the inner wall of the kettle body is provided with a plurality of second grinding protrusions.
7. The method according to claim 6, wherein a first hinge is provided on the rotating shaft, a first piston is provided on the first hinge, a first piston is provided on one side of the first piston close to the stirring plate, a piston shaft is provided on one side of the first piston close to the stirring plate, a second piston is provided on one side of the piston shaft close to the stirring plate, a second hinge is provided on the stirring plate, the second piston is rotatably mounted on the second hinge, a second spring is provided between the first piston and the second piston, and the second spring is sleeved on the periphery of the piston shaft.
8. The method for preparing the bio-based modified low-heat-generation reinforcing agent according to claim 6, wherein the gap between the second grinding protrusion and the inner wall of the kettle body is m, and m is more than 0 and less than or equal to 2 cm.
9. The method for preparing the bio-based modified low-heat-generation reinforcing agent according to claim 6, wherein the included angle between the stirring plate and the vertical direction is alpha, and is more than or equal to 30 degrees and less than or equal to 80 degrees.
10. The method for preparing the bio-based modified low-heat-generation reinforcing agent according to claim 4, wherein a stirring blade is arranged on the periphery of the rotating shaft, a plurality of shunting holes are formed in the stirring blade, a guide shaft sleeve is further arranged on the periphery of the rotating shaft, a mounting disc located in the kettle cavity is arranged on the guide shaft sleeve, and a through hole is formed in the mounting disc.
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