CN112048110A - Mixed rubber and preparation method thereof - Google Patents
Mixed rubber and preparation method thereof Download PDFInfo
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- CN112048110A CN112048110A CN202010955517.1A CN202010955517A CN112048110A CN 112048110 A CN112048110 A CN 112048110A CN 202010955517 A CN202010955517 A CN 202010955517A CN 112048110 A CN112048110 A CN 112048110A
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- carbon black
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- latex
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 71
- 239000005060 rubber Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000006229 carbon black Substances 0.000 claims abstract description 106
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 51
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 40
- 229920000126 latex Polymers 0.000 claims abstract description 37
- 239000004816 latex Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 239000007822 coupling agent Substances 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims description 53
- 238000003756 stirring Methods 0.000 claims description 38
- 239000011259 mixed solution Substances 0.000 claims description 30
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 244000043261 Hevea brasiliensis Species 0.000 claims description 15
- 229920003052 natural elastomer Polymers 0.000 claims description 15
- 229920001194 natural rubber Polymers 0.000 claims description 15
- 238000003825 pressing Methods 0.000 claims description 15
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 239000010692 aromatic oil Substances 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 8
- 239000011593 sulfur Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 239000004310 lactic acid Substances 0.000 claims description 6
- 235000014655 lactic acid Nutrition 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 230000001112 coagulating effect Effects 0.000 claims description 5
- 239000004014 plasticizer Substances 0.000 claims description 5
- 239000003755 preservative agent Substances 0.000 claims description 5
- 230000002335 preservative effect Effects 0.000 claims description 5
- 230000000903 blocking effect Effects 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 4
- 239000000080 wetting agent Substances 0.000 claims description 4
- 229920006173 natural rubber latex Polymers 0.000 claims description 3
- 238000004073 vulcanization Methods 0.000 claims description 3
- 230000003311 flocculating effect Effects 0.000 claims description 2
- 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 1
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 238000009736 wetting Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 8
- 238000001238 wet grinding Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 10
- 239000000945 filler Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- STSDHUBQQWBRBH-UHFFFAOYSA-N n-cyclohexyl-1,3-benzothiazole-2-sulfonamide Chemical compound N=1C2=CC=CC=C2SC=1S(=O)(=O)NC1CCCCC1 STSDHUBQQWBRBH-UHFFFAOYSA-N 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 4
- 238000007580 dry-mixing Methods 0.000 description 4
- 239000012744 reinforcing agent Substances 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- HNWAHFPYJHAAJE-UHFFFAOYSA-N n-tert-butyl-1,3-benzothiazole-2-sulfonamide Chemical compound C1=CC=C2SC(S(=O)(=O)NC(C)(C)C)=NC2=C1 HNWAHFPYJHAAJE-UHFFFAOYSA-N 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 238000010074 rubber mixing Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010057 rubber processing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 230000004580 weight loss Effects 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
- C08L7/00—Compositions of natural rubber
- C08L7/02—Latex
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
- B29B7/7476—Systems, i.e. flow charts or diagrams; Plants
- B29B7/7495—Systems, i.e. flow charts or diagrams; Plants for mixing rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/22—Component parts, details or accessories; Auxiliary operations
- B29B7/28—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/22—Component parts, details or accessories; Auxiliary operations
- B29B7/28—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
- B29B7/283—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control measuring data of the driving system, e.g. torque, speed, power
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/22—Component parts, details or accessories; Auxiliary operations
- B29B7/28—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
- B29B7/286—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control measuring properties of the mixture, e.g. temperature, density
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/88—Adding charges, i.e. additives
- B29B7/90—Fillers or reinforcements, e.g. fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
- B60C1/0016—Compositions of the tread
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
- B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
- B29B7/18—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft
- B29B7/183—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft having a casing closely surrounding the rotors, e.g. of Banbury type
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a mixed rubber and a preparation method thereof, belonging to the technical field of rubber material treatment and comprising the following raw materials in parts by mass: 10-25 parts of white carbon black, 80-120 parts of natural latex, 1-3 parts of a pretreated liquid coupling agent, 0.5-1.5 parts of a treating agent, 3-5 parts of an anti-aging agent, 2-3 parts of a tackifier and the balance of deionized water, and pretreating the natural latex according to the following steps; preparing white carbon black aqueous dispersion; preparing a latex and white carbon black composite material; the rubber compound prepared by the method has the special performances of wet grinding, tear resistance, anti-chipping and anti-pricking, is easy to process, and has wide market prospect.
Description
Technical Field
The invention belongs to the technical field of rubber material treatment, and particularly relates to a mixed rubber and a preparation method thereof.
Background
In the rubber material processing process, mixing is the most critical process, and dozens of compounding agents such as natural rubber, synthetic rubber, reinforcing materials, vulcanizing materials, anti-aging materials and the like are uniformly mixed through mixing to prepare a mixed rubber material which becomes a raw material for producing various rubber products, so that the processing performance of the rubber product and various service performances of the product are directly influenced by the mixed rubber performance and the mixing process. The mixing process is also the highest energy consumption procedure in rubber processing, and accounts for 40% of the total energy consumption in the tire production process. However, the rubber industry in China still uses a mechanical dry mixing method with high energy consumption, long industrial chain and poor environmental protection, rubber/filler/compounding agent are mixed in an internal mixer in a multi-stage way, the power consumption of each ton of mixed rubber is about 400 kW.H, the annual power consumption is averagely 50 hundred million kW.H, and the annual power consumption is about 40 million yuan. Therefore, the innovation and the modification of the mixing process and the development of the energy-saving mixing process become important for energy-saving measures in the rubber industry. The innovation of the mixing process is mainly to develop the current batch mixing method into the continuous mixing method, wherein the low-temperature one-step mixing and wet mixing technology is the process technology with the best development prospect and the most obvious energy-saving effect. Other mixing techniques include a tandem internal mixer and screw extrusion. The tread rubber used by the engineering tire has harsh use conditions and poor road surface environment, and the rubber manufactured by the traditional process can not meet the use requirements of the tire increasingly, so that the quality problems of early damage and the like of the tire are caused, therefore, the invention of the rubber compound used for the engineering tire has important significance.
Disclosure of Invention
Aiming at various defects in the prior art, the mixing rubber and the preparation method thereof are provided.
The invention relates to a mixing process combining a white carbon black wet mixing technology and a dry technology, wherein the wet mixing technology is a method for producing rubber mixing rubber by preparing water dispersion from fillers such as carbon black, white carbon black and the like which are processed in advance, fully mixing the water dispersion with rubber latex in a liquid state, and then coagulating, dehydrating, drying and the like. The method is completely different from the traditional method of mixing dry rubber, carbon black, white carbon black and other compounding agents in an internal mixer by a multi-stage dry method. Natural latex is a suspension of rubber micelle particles in water, the outermost part of the rubber micelle particles being a protective layer consisting of proteins and lipids. The substances in the protective layer all have the function of a surfactant. Active reinforcing agents such as white carbon black and carbon black absorb the surfactants in a liquid state, the surfactants are inactivated, the formation of a reinforcing mechanism between the reinforcing agents and rubber is prevented, the reinforcing agents are often not matched with the settling velocity of latex due to different polarities and specific gravities, and the reinforcing agents are not easy to be uniformly dispersed in a latex system, so that the performance of the rubber is often damaged.
Adding a certain proportion of water into fillers such as carbon black, white carbon black and the like which are processed in advance to uniformly disperse the fillers, adding raw materials such as carbon black, anti-aging agents and the like of different types into an F110 internal mixer to carry out dry mixing, and preparing the tread mixing masterbatch for the engineering tires with different performance requirements.
In order to achieve the purpose, the invention provides the following technical scheme:
the mixing rubber is prepared from the following raw materials in parts by mass: 10-25 parts of white carbon black, 80-120 parts of natural latex, 1-3 parts of a pretreated liquid coupling agent, 0.5-1.5 parts of a treating agent, 3-5 parts of an anti-aging agent, 2-3 parts of a tackifier and the balance of deionized water.
Preferably, the pretreated liquid coupling agent comprises Si747, the dispersing agent comprises FS-78T, the moistening agent comprises Neoresin, and the anti-settling agent comprises S-8021.
Preferably, the dispersing agent, the moistening agent and the anti-settling agent are mixed according to the weight ratio of 0.8-1: 1.5-2: mixing at a ratio of 1.5-2.
A method for preparing a rubber composition as described above, comprising the steps of:
s1: pretreating natural latex;
s2: preparing white carbon black aqueous dispersion;
s3: preparing a latex and white carbon black composite material;
s4: and (3) mixing the latex and the white carbon black composite material to prepare the rubber compound.
Preferably, in step S1, the pretreatment of the natural rubber latex comprises the steps of: adding ammonia accounting for 0.5-1.5 percent of the weight of fresh latex into the fresh latex which is just collected as a preservative, adding lactic acid accounting for 1-1.5 percent of the weight of the fresh latex, neutralizing the ammonia and coagulating the latex, wherein the added lactic acid enables rubber particles to form hydrophilic groups, and the rubber particles and water form a hydration state, thereby leading the latex to be gelled and solidified.
Preferably, in step S2, adding white carbon black into a stirring kettle, adding deionized water, stirring to obtain a white carbon black mixed solution, and ball-milling the white carbon black mixed solution for 2-6 hours to obtain the white carbon black aqueous dispersion, wherein the weight ratio of white carbon black to deionized water is 1: 2-1: 5.
preferably, in step S3, the preparation of the latex and white carbon black composite material includes the following steps:
step a: natural latex/white carbon black mixed liquor
Mixing the pretreated liquid coupling agent and the white carbon black aqueous dispersion according to the ratio of 1: 20-1: 10, stirring and mixing, adding the natural latex, and stirring uniformly;
step b: b, adding hydrochloric acid with the concentration of 10% -30% into the natural latex/white carbon black mixed solution prepared in the step a, stirring, and sequentially adding an anti-aging agent and a tackifier during stirring;
step c: preparation of Natural rubber/white carbon Black masterbatch
And c, drying and flocculating the substance obtained in the step b, drying in an oven at the temperature of 60-100 ℃, preparing the natural latex/white carbon black mixed solution into a flaky solid structure by using tabletting equipment, and performing sheet stacking and blocking to obtain the natural rubber/white carbon black master batch.
Preferably, in the step b, 1/150-1/50 of hydrochloric acid is added, wherein the weight of the hydrochloric acid accounts for the total weight of the natural latex/white carbon black mixed solution, the stirring speed is 60-120rpm, and the stirring time is 2.5-4.5 h.
Preferably, step S4 includes the steps of:
step I: mixing natural rubber/white carbon black master batch, carbon black, an anti-aging agent and a plasticizer in an internal mixer, adding aromatic oil 5-15phr after pressing for 30-50s, lifting a top plug after pressing for 30-50s, cleaning, discharging rubber after pressing for 20-40s to the temperature of 150 ℃ and 170 ℃, and preparing a section of master batch;
step II: adding sulfur and promoter into the first-stage masterbatch, mixing, pressurizing to 100 deg.C, discharging rubber after 90-120s, and making into mixed rubber.
Preferably, in the step I, the sulfur and the accelerator respectively account for 0.5-1.5% and 0.3-0.7% of the weight of the first section of masterbatch, and the accelerator comprises a vulcanization accelerator which is N-tert-butyl-2-benzothiazole sulfonamide or N-cyclohexyl-2-benzothiazole sulfonamide.
The invention has the beneficial effects that:
the product produced by the method has the advantages of special performances of wet grinding resistance, tear resistance, anti-chipping and anti-pricking, easy processing, stable quality batch and the like. The white carbon black, the carbon black and other fillers are added into the mixing rubber in certain parts, so that the dispersibility of the fillers and the tear resistance of the rubber are further improved.
The method overcomes the defect of dry mixing, and the natural rubber/white carbon black wet masterbatch can obviously reduce the rolling resistance of the tire and is a preferred material for manufacturing green tires.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
The first embodiment is as follows:
the mixing rubber is prepared from the following raw materials in parts by mass: 10 parts of white carbon black, 80 parts of natural latex, 1 part of pretreated liquid coupling agent, 0.5 part of treating agent, 3 parts of anti-aging agent, 2 parts of tackifier and the balance of deionized water. The treating agent comprises a mixture of a dispersing agent, a wetting agent and an anti-settling agent, wherein the dispersing agent: cleaning and moistening agents: the anti-settling agent is 0.8: 1.5: 1.5.
the pretreated liquid coupling agent comprises Si747, the dispersing agent comprises FS-78T, the moistening agent comprises Neoresin, and the anti-settling agent comprises S-8021.
A method for preparing a rubber compound comprises the following steps:
s1: pretreating natural latex;
adding 0.5% of ammonia by weight of fresh latex into fresh latex which is just collected as a preservative, adding 1% of lactic acid by weight of the fresh latex, neutralizing the ammonia and coagulating the latex. The added lactic acid forms hydrophilic groups on the rubber particles, so that the rubber particles and water form a hydrated state, and the latex is gelled and solidified.
S2: preparation of white carbon black aqueous dispersion
Adding white carbon black into a stirring kettle, adding deionized water and stirring to prepare a white carbon black mixed solution, and performing ball milling on the white carbon black mixed solution for 2 hours to prepare a white carbon black water dispersion, wherein the weight ratio of the white carbon black to the deionized water is 1: 2.
s3: the preparation of the latex and white carbon black composite material comprises the following steps:
mixing the pretreated liquid coupling agent and the white carbon black aqueous dispersion according to the ratio of 1: 20, adding the natural latex, and uniformly stirring to obtain a natural latex/white carbon black mixed solution;
adding hydrochloric acid with the concentration of 10% into the prepared natural latex/white carbon black mixed solution, stirring, adding 1/150 of which the weight of the hydrochloric acid accounts for the total weight of the natural latex/white carbon black mixed solution, wherein the stirring speed is 60rpm, and the stirring time is 2.5h, and sequentially adding an anti-aging agent and a tackifier during the stirring process to obtain the natural latex/white carbon black mixed solution;
and then, carrying out drying flocculation treatment on the obtained substances, namely drying the substances in an oven at 60 ℃ for 5 hours, preparing the natural latex/white carbon black mixed solution into a flaky solid structure through a tabletting device, and carrying out sheet stacking and blocking to obtain the natural rubber/white carbon black master batch.
Step S4 includes the following steps:
and (2) mixing the natural rubber/white carbon black master batch prepared in the step S3 with carbon black, an anti-aging agent and a plasticizer in an internal mixer, adding aromatic oil after pressing for 30S, wherein the adding amount of the aromatic oil is 5phr, lifting a top plug after pressing for 30S, cleaning, pressing for 20S to 150 ℃, and discharging rubber to prepare a section of master batch.
Adding sulfur accounting for 0.5 percent of the weight of the first-stage masterbatch and an accelerator accounting for 0.3 percent of the weight of the first-stage masterbatch into the prepared first-stage masterbatch for mixing, pressurizing to 100 ℃, discharging after 90s, and obtaining the rubber compound. The accelerator adopts a vulcanization accelerator which is N-tertiary butyl-2-benzothiazole sulfonamide (NS).
Example two
The mixing rubber is prepared from the following raw materials in parts by mass: 25 parts of white carbon black, 120 parts of natural latex, 3 parts of pretreated liquid coupling agent, 1.5 parts of treating agent, 5 parts of anti-aging agent, 3 parts of tackifier and the balance of deionized water. The treating agent comprises a mixture of a dispersing agent, a wetting agent and an anti-settling agent, wherein the dispersing agent: cleaning and moistening agents: the anti-settling agent is 1: 2: 2. the pretreated liquid coupling agent comprises Si747, the dispersing agent comprises FS-78T, the moistening agent comprises Neoresin, and the anti-settling agent comprises S-8021.
A method for preparing a rubber compound comprises the following steps:
s1: pretreatment of natural rubber latex
Ammonia accounting for 1.5 percent of the mass of the fresh latex is added into the fresh latex which is just collected to be used as a preservative, lactic acid accounting for 1.5 percent of the mass of the fresh latex is added, and the ammonia is neutralized and the latex is coagulated. The added acid forms hydrophilic groups on the rubber particles, so that the rubber particles and water form a hydrated state, thereby gelling and curing the latex.
S2: preparation of white carbon black aqueous dispersion
Adding white carbon black into a stirring kettle, adding deionized water and stirring to prepare a white carbon black mixed solution, and performing ball milling on the white carbon black mixed solution for 6 hours to prepare a white carbon black water dispersion, wherein the weight ratio of the white carbon black to the deionized water is 1: 5.
s3: the preparation of the latex and white carbon black composite material comprises the following steps:
mixing the pretreated liquid coupling agent and the white carbon black aqueous dispersion according to the ratio of 1: 10, stirring and mixing, adding the natural latex, and uniformly stirring to obtain a natural latex/white carbon black mixed solution;
adding hydrochloric acid with the concentration of 30% into the prepared natural latex/white carbon black mixed solution, stirring, adding 1/50 of which the weight of the hydrochloric acid accounts for the total weight of the natural latex/white carbon black mixed solution, wherein the stirring speed is 120rpm, and the stirring time is 4.5h, and sequentially adding an anti-aging agent and a tackifier during the stirring process to obtain the natural latex/white carbon black mixed solution; and then, carrying out drying flocculation treatment on the obtained substances, drying in an oven at 100 ℃, preparing the natural latex/white carbon black mixed solution into a flaky solid structure through a tabletting device, and carrying out sheet stacking and blocking to obtain the natural rubber/white carbon black masterbatch.
Step S4 includes the following steps:
mixing the prepared natural rubber/white carbon black master batch with carbon black, an anti-aging agent and a plasticizer in an internal mixer, adding aromatic oil after pressing for 50s, adding the aromatic oil in an amount of 15phr, lifting a top plug after pressing for 50s, cleaning, pressing for 40s to 170 ℃, and discharging rubber to prepare a section of master batch.
Adding sulfur accounting for 1.5 percent of the weight of the primary rubber and an accelerator accounting for 0.7 percent of the weight of the primary rubber into the prepared primary rubber, mixing, pressurizing to 100 ℃, discharging rubber after 120s, and obtaining the rubber compound. The accelerator adopts N-cyclohexyl-2-benzothiazole sulfonamide (CZ).
EXAMPLE III
The mixing rubber is prepared from the following raw materials in parts by mass: 20 parts of white carbon black, 100 parts of natural latex, 2 parts of pretreated liquid coupling agent, 1 part of treating agent, 4 parts of anti-aging agent, 2.5 parts of tackifier and the balance of deionized water. The treating agent comprises a mixture of a dispersing agent, a wetting agent and an anti-settling agent, wherein the dispersing agent: cleaning and moistening agents: the anti-settling agent is 0.9: 1.7: 1.8. the pretreated liquid coupling agent comprises Si747, the dispersing agent comprises FS-78T, the moistening agent comprises Neoresin, and the anti-settling agent comprises S-8021.
A method for preparing a rubber compound comprises the following steps:
s1: pretreating natural latex;
adding ammonia accounting for 1 percent of the weight of the fresh latex into the fresh latex which is just collected as a preservative, adding lactic acid accounting for 1.2 percent of the weight of the fresh latex, neutralizing the ammonia and coagulating the latex. The added acid forms hydrophilic groups on the rubber particles, so that the rubber particles and water form a hydrated state, thereby gelling and curing the latex.
S2: preparation of white carbon black aqueous dispersion
Adding white carbon black into a stirring kettle, adding deionized water and stirring to prepare a white carbon black mixed solution, and performing ball milling on the white carbon black mixed solution for 5 hours to prepare a white carbon black water dispersion, wherein the weight ratio of the white carbon black to the deionized water is 1: 3.
s3: the preparation of the latex and white carbon black composite material comprises the following steps:
mixing the pretreated liquid coupling agent and the white carbon black aqueous dispersion according to the ratio of 1: 15, stirring and mixing, adding the natural latex, and uniformly stirring to obtain a natural latex/white carbon black mixed solution;
adding hydrochloric acid with the concentration of 20% into the prepared natural latex/white carbon black mixed solution, stirring, adding 1/100 of which the weight of the hydrochloric acid accounts for the total weight of the natural latex/white carbon black mixed solution, wherein the stirring speed is 100rpm, the stirring time is 3 hours, and sequentially adding an anti-aging agent and a tackifier during the stirring process to obtain the natural latex/white carbon black mixed solution; and then the obtained substances are subjected to drying flocculation treatment, dried in an oven at the temperature of 80 ℃, and then the natural latex/white carbon black mixed solution is made into a flaky solid structure by a tabletting device, and is piled and briquetted to obtain the natural rubber/white carbon black masterbatch.
Step S4 includes the following steps:
mixing the prepared natural rubber/white carbon black master batch with carbon black, an anti-aging agent and a plasticizer in an internal mixer, adding aromatic oil after pressing for 40s, adding 10phr of aromatic oil, lifting a top plug after pressing for 40s, cleaning, pressing for 30s to 160 ℃, and discharging rubber to prepare a section of master batch.
Adding sulfur and an accelerator into the prepared primary rubber, mixing, pressurizing to 100 ℃, discharging rubber after 100s, and thus obtaining the rubber compound. The sulfur and the accelerator respectively account for 1 percent and 0.5 percent of the weight of the first section of the masterbatch, and the accelerator adopts N-cyclohexyl-2-benzothiazole sulfonamide (CZ).
Experimental examples
The traditional dry rubber mixing is that raw materials such as natural rubber, carbon black, white carbon black, an anti-aging agent and the like are mechanically mixed in an internal mixer device in a solid state. During mechanical mixing, rubber molecular weight is broken to varying degrees due to shear heating, resulting in a decrease in performance. The wet mixing process fundamentally solves the problem and ensures the physical properties of the rubber material.
The table shows the experimental record of the performance of the product prepared by the traditional dry mixing method and the wet mixing process of the invention
Watch 1
| Item | Conventional dry process | Wet mixing process | The lifting rate% |
| Tensile strength, MPa | 22.4 | 23.7 | 6％ |
| Elongation at break,% | 526 | 584 | 11％ |
| Modulus of elasticity, MPa | 2.1 | 2.6 | 24％ |
| Shore A hardness | 62 | 63 | 1％ |
| Tear Strength KN/m | 82 | 115 | 40％ |
| Rebound value% | 31 | 33 | 6％ |
| Akron abrasion (cm)3) | 0.184 | 0.164 | 10％ |
| Cutting weight loss/g | 1.286 | 1.216 | 5％ |
As can be seen from the table I, compared with the traditional dry-method mixing process, the wet-method mixing process has the advantages that the tensile strength is improved by 6%, the tearing strength is improved by 40%, the cutting resistance is improved by 5%, the wear resistance is improved by 10%, and the use requirements can be well met.
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. The mixing rubber is characterized by comprising the following raw materials in parts by mass: 10-25 parts of white carbon black, 80-120 parts of natural latex, 1-3 parts of a pretreated liquid coupling agent, 0.5-1.5 parts of a treating agent, 3-5 parts of an anti-aging agent, 2-3 parts of a tackifier and the balance of deionized water.
2. A rubber composition as claimed in claim 1, wherein said pre-treated liquid coupling agent comprises Si747, dispersing agent comprises FS-78T, wetting agent comprises NeoResin, and anti-settling agent comprises S-8021.
3. A rubber composition according to claim 2, wherein the dispersing, wetting and anti-settling agents are present in a ratio of 0.8 to 1: 1.5-2: 1.5-2.
4. A method for preparing a rubber composition as claimed in claim 1, characterized in that it comprises the following steps:
s1: pretreating natural latex;
s2: preparing white carbon black aqueous dispersion;
s3: preparing a latex and white carbon black composite material;
s4: and (3) mixing the latex and the white carbon black composite material to prepare the rubber compound.
5. The method according to claim 4, wherein the step S1, the natural rubber latex pre-treatment comprises the steps of: adding ammonia accounting for 0.5-1.5 percent of the weight of the fresh latex into the fresh latex which is just collected as a preservative, adding lactic acid accounting for 1-1.5 percent of the weight of the fresh latex, neutralizing the ammonia and coagulating the latex.
6. The preparation method according to claim 4, wherein in step S2, the white carbon black is added into a stirring kettle, the deionized water is added and stirred to prepare a white carbon black mixed solution, and the white carbon black mixed solution is ball-milled for 2-6 hours to prepare the white carbon black aqueous dispersion, wherein the weight ratio of the white carbon black to the deionized water is 1: 2-1: 5.
7. the preparation method according to claim 4, wherein in the step S3, the preparation of the latex and white carbon black composite material comprises the following steps:
step a: natural latex/white carbon black mixed liquor
Mixing the pretreated liquid coupling agent and the white carbon black aqueous dispersion according to the ratio of 1: 20-1: 10, stirring and mixing, adding the natural latex, and stirring uniformly;
step b: b, adding hydrochloric acid with the concentration of 10% -30% into the natural latex/white carbon black mixed solution prepared in the step a, stirring, and sequentially adding an anti-aging agent and a tackifier during stirring;
step c: preparation of Natural rubber/white carbon Black masterbatch
And c, drying and flocculating the substance obtained in the step b, drying in an oven at the temperature of 60-100 ℃, preparing the natural latex/white carbon black mixed solution into a flaky solid structure by using tabletting equipment, and performing sheet stacking and blocking to obtain the natural rubber/white carbon black master batch.
8. The preparation method according to claim 7, wherein in the step b, the hydrochloric acid is added in an amount of 1/150-1/50 based on the total weight of the natural latex/silica mixture, the stirring speed is 60-120rpm, and the stirring time is 2.5-4.5 h.
9. The method according to claim 4, wherein the step S4 includes the steps of:
step I: mixing natural rubber/white carbon black master batch, carbon black, an anti-aging agent and a plasticizer in an internal mixer, adding aromatic oil 5-15phr after pressing for 30-50s, lifting a top plug after pressing for 30-50s, cleaning, discharging rubber after pressing for 20-40s to the temperature of 150 ℃ and 170 ℃, and preparing a section of master batch;
step II: adding sulfur and promoter into the first-stage masterbatch, mixing, pressurizing to 100 deg.C, discharging rubber after 90-120s, and making into mixed rubber.
10. The preparation method according to claim 9, wherein in step i, the sulfur and the accelerator respectively account for 0.5-1.5% and 0.3-0.7% of the weight of the primary rubber, and the accelerator comprises a vulcanization accelerator selected from the group consisting of N-tert-butyl-2-benzothiazolesulfenamide and N-cyclohexyl-2-benzothiazolesulfenamide.
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