All-steel tire inner liner rubber and preparation method thereof

By introducing the nano-inorganic reinforcement RC-15 and the second-stage mixing process into the tire airtight layer glue, the problems of large heat generation and unstable airtightness caused by excessive carbon black use are solved, and the airtightness improvement and cost reduction are achieved, while maintaining the stability and environmental protection of the glue.

CN120484394APending Publication Date: 2025-08-15JIANGSU GENERAL SCI TECH
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Patent Information

Application Number
CN202510718351.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-30
Publication Date
2025-08-15

AI Technical Summary

Technical Problem

Too high amount of carbon black in traditional tire airtight layer rubber leads to large heat generation and poor dynamic performance. Too much plasticizer affects airtightness, and uneven dispersion of coarse particle fillers leads to unstable airtightness.

Method used

A nano-scale inorganic reinforcement was introduced, and a nano-inorganic reinforcement RC-15, with a sheet-layer structure, combined with a two-stage mixing process, blocking the gas penetration path through the maze effect, and preparing an all-steel tire air-tight layer glue.

Benefits of technology

Significantly improve airtightness and fatigue resistance, reduce the cost of formula raw materials, and maintain the stability and environmental protection of the rubber processing.

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Abstract

The invention provides all-steel tire inner liner rubber and a preparation method thereof, and belongs to the technical field of rubber. The all-steel tire inner liner rubber is prepared from the following components in parts by weight: 70 to 85 parts of butyl rubber, 25 to 45 parts of butyl reclaimed rubber, 3 to 5 parts of natural rubber, 45 to 55 parts of carbon black N660, 8 to 20 parts of nano inorganic reinforcing agent, 3 to 8 parts of oil, 0.4 to 0.6 part of stearic acid, 4 to 6 parts of C5 resin, 2 to 6 parts of tackifying resin, 8 to 12 parts of homogenizing agent, 0.2 to 0.4 part of magnesium oxide, 0.4 to 0.6 part of sulfur powder, 1.1 to 1.6 parts of accelerant and 0.7 to 1.4 parts of zinc oxide. The nano lamellar structure of the nano-scale inorganic reinforcing agent is used for remarkably improving the air tightness, the fatigue flex resistance and the mechanical property of the airtight layer, meanwhile, the raw material cost of the formula can be reduced, and the processing stability and the environmental protection property of the rubber material can be kept.
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Description

Technical Field

[0001] The invention belongs to the technical field of rubber, and in particular relates to an all-steel tire airtight layer rubber and a preparation method thereof. Background Art

[0002] Traditional tire innerliners often use a high proportion of carbon black filler to improve air tightness and mechanical properties, but there are the following problems: excessive carbon black dosage leads to high heat generation and poor dynamic performance of the rubber compound; air tightness decreases significantly when the plasticizer dosage exceeds 10phr; coarse particle fillers are unevenly dispersed, resulting in unstable air tightness. Summary of the Invention

[0003] The present invention aims to overcome the shortcomings of the prior art and provide an all-steel tire innerliner adhesive and its preparation method. By introducing a nano-scale inorganic reinforcing agent, the lamellar structure of which blocks gas permeation paths through a "maze effect," combined with a two-stage mixing process, an economical and environmentally friendly innerliner adhesive is produced. This significantly improves the airtightness, fatigue resistance, and mechanical properties of the innerliner. Furthermore, the addition of the nano-inorganic reinforcing agent RC-15 reduces the rubber content of the formulation, lowering the raw material cost while maintaining the processing stability and environmental friendliness of the rubber.

[0004] To achieve the above technical objectives, the technical solutions adopted in the embodiments of the present invention are: In a first aspect, an embodiment of the present invention provides an all-steel tire innerliner rubber, comprising the following components, in parts by weight: 70-85 parts of butyl rubber, 25-45 parts of butyl reclaimed rubber, 3-5 parts of natural rubber, 45-55 parts of carbon black N660, 8-20 parts of a nano-inorganic reinforcing agent, 3-8 parts of oil, 0.4-0.6 parts of stearic acid, 4-6 parts of C5 resin, 2-6 parts of a tackifying resin, 8-12 parts of a leveling agent, 0.2-0.4 parts of magnesium oxide, 0.4-0.6 parts of sulfur powder, 1.1-1.6 parts of an accelerator, and 0.7-1.4 parts of zinc oxide.

[0005] Furthermore, the nano inorganic reinforcing agent is a silicate material with a sheet thickness of less than 100 nm, a specific surface area of ≥200 m² / g, and complies with REACH environmental protection standards.

[0006] Furthermore, the oil is environmentally friendly aromatic oil or naphthenic oil.

[0007] Furthermore, the C5 resin is hydrogenated C5 petroleum resin.

[0008] Furthermore, the tackifying resin is octylphenol formaldehyde tackifying resin.

[0009] Furthermore, the butyl rubber includes brominated butyl rubber or chlorinated butyl rubber.

[0010] Furthermore, the homogenizer is a hydrocarbon resin mixture 40MSF.

[0011] Furthermore, the accelerator is dibenzothiazyl disulfide.

[0012] In a second aspect, an embodiment of the present invention provides a method for preparing the all-steel tire innerliner adhesive described in the first aspect, comprising the following steps: (1) One-stage mixing: 70-85 parts of butyl rubber, 25-45 parts of butyl reclaimed rubber, 3-5 parts of natural rubber, 45-55 parts of carbon black N660, 8-20 parts of nano-inorganic reinforcing agent, 3-8 parts of oil, 0.4-0.6 parts of stearic acid, 4-6 parts of C5 resin, 2-6 parts of tackifying resin, 8-12 parts of homogenizer and 0.2-0.4 parts of magnesium oxide are put into an internal mixer, the upper bolt pressure is 0.4-0.59 MPa, the rotor speed is 25-50 r / min, the discharge temperature is 120-140°C, and the mixing time is 140-190 s to obtain a one-stage mixed rubber; (2) Second stage mixing: the first stage mixed rubber obtained in step (1), 0.4-0.6 parts of sulfur powder, 1.1-1.6 parts of accelerator and 0.7-1.4 parts of zinc oxide are put into an internal mixer with a rotor speed of 22-30 r / min, a top bolt pressure of 0.4-0.59 MPa, a discharge temperature of 98-110°C and a mixing time of 80-120 s to obtain an airtight layer rubber.

[0013] The technical solution provided by the embodiment of the present invention has the following beneficial effects: The present invention achieves the following functions by introducing a nano-scale inorganic reinforcing agent with a lamellar structure of less than 100 nanometers in thickness and blocking the gas permeation path through a "maze effect" combined with a two-stage mixing process: Improved air tightness: The nanosheet layer (thickness <100nm) of the nano-inorganic reinforcing agent RC-15 increases the gas penetration path. After adding a certain amount of this material to the airtight layer formula, the air tightness of the rubber compound is significantly improved.

[0014] Cost reduction: Adding 8 to 20 parts of nano inorganic reinforcing agent RC-15 to the rubber formula can reduce the rubber content of the formula and reduce the cost of raw materials.

[0015] Environmental protection: Nano inorganic reinforcing agent RC-15 does not contain PAHS and heavy metals and complies with REACH standards. DETAILED DESCRIPTION

[0016] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0017] Example 1 A method for preparing an all-steel tire innerliner adhesive comprises the following steps: (1) One-stage mixing: by weight, 77 parts of butyl rubber BIIR-2302, 40 parts of butyl reclaimed rubber, 3 parts of natural rubber, 55 parts of carbon black N660, 8 parts of nano-inorganic reinforcing agent RC-15, 6.5 parts of naphthenic oil, 0.5 parts of stearic acid 1842 type, 5 parts of C5 resin A-100, 4 parts of tackifying resin SL1802, 9.41 parts of homogenizing agent 40MSF and 0.25 parts of magnesium oxide MAGCHEM 40 were put into an internal mixer with a top bolt pressure of 0.55 MPa, a rotor speed of 30 r / min, a discharge temperature of 125 °C and a mixing time of 160 s to obtain a one-stage mixed rubber; (2) Second stage mixing: put the first stage mixed rubber, 0.5 parts of sulfur powder, 1.5 parts of accelerator MBTS and 1.25 parts of zinc oxide into an internal mixer, with a rotor speed of 25 r / min, a top bolt pressure of 0.55 MPa, a rubber discharge temperature of 107°C and a mixing time of 105 s to obtain the airtight layer rubber.

[0018] Example 2 A method for preparing an all-steel tire innerliner adhesive comprises the following steps: (1) One-stage mixing: by weight, 77 parts of butyl rubber BIIR-2302, 40 parts of butyl reclaimed rubber, 3 parts of natural rubber, 55 parts of carbon black N660, 10 parts of nano-inorganic reinforcing agent RC-15, 6.5 parts of naphthenic oil, 0.5 parts of stearic acid 1842 type, 5 parts of C5 resin A-100, 4 parts of tackifying resin SL1802, 9.41 parts of homogenizing agent 40MSF and 0.25 parts of magnesium oxide MAGCHEM 40 were put into an internal mixer with a top bolt pressure of 0.55 MPa, a rotor speed of 30 r / min, a discharge temperature of 125 °C and a mixing time of 160 s to obtain a one-stage mixed rubber; (2) Second stage mixing: put the first stage mixed rubber, 0.5 parts of sulfur powder, 1.5 parts of accelerator MBTS and 1.25 parts of zinc oxide into an internal mixer, with a rotor speed of 25 r / min, a top bolt pressure of 0.55 MPa, a rubber discharge temperature of 107°C and a mixing time of 105 s to obtain the airtight layer rubber.

[0019] Example 3 A method for preparing an all-steel tire innerliner adhesive comprises the following steps: (1) One-stage mixing: by weight, 77 parts of butyl rubber BIIR-2302, 40 parts of butyl reclaimed rubber, 3 parts of natural rubber, 55 parts of carbon black N660, 14 parts of nano-inorganic reinforcing agent RC-15, 6.5 parts of naphthenic oil, 0.5 parts of stearic acid 1842 type, 5 parts of C5 resin A-100, 4 parts of tackifying resin SL1802, 9.41 parts of homogenizing agent 40MSF and 0.25 parts of magnesium oxide MAGCHEM 40 were put into an internal mixer with a top bolt pressure of 0.55 MPa, a rotor speed of 30 r / min, a discharge temperature of 125 °C and a mixing time of 160 s to obtain a one-stage mixed rubber; (2) Second stage mixing: put the first stage mixed rubber, 0.5 parts of sulfur powder, 1.5 parts of accelerator MBTS and 1.25 parts of zinc oxide into an internal mixer, with a rotor speed of 25 r / min, a top bolt pressure of 0.55 MPa, a rubber discharge temperature of 107°C and a mixing time of 105 s to obtain the airtight layer rubber.

[0020] Example 4 A method for preparing an all-steel tire innerliner adhesive comprises the following steps: (1) One-stage mixing: by weight, 77 parts of butyl rubber BIIR-2302, 40 parts of butyl reclaimed rubber, 3 parts of natural rubber, 55 parts of carbon black N660, 18 parts of nano-inorganic reinforcing agent RC-15, 6.5 parts of oil-naphthenic oil, 0.5 parts of stearic acid 1842 type, 5 parts of C5 resin A-100, 4 parts of tackifying resin SL1802, 9.41 parts of homogenizing agent 40MSF and 0.25 parts of magnesium oxide MAGCHEM 40 were put into an internal mixer with a top bolt pressure of 0.55 MPa, a rotor speed of 30 r / min, a discharge temperature of 125 ° C, and a mixing time of 160 s to obtain a one-stage mixed rubber; (2) Second stage mixing: put the first stage mixed rubber, 0.5 parts of sulfur powder, 1.5 parts of accelerator MBTS and 1.25 parts of zinc oxide into an internal mixer, with a rotor speed of 25 r / min, a top bolt pressure of 0.55 MPa, a rubber discharge temperature of 107°C and a mixing time of 105 s to obtain the airtight layer rubber.

[0021] Example 5 A method for preparing an all-steel tire innerliner adhesive comprises the following steps: (1) One-stage mixing: by weight, 77 parts of butyl rubber BIIR-2302, 40 parts of butyl reclaimed rubber, 3 parts of natural rubber, 55 parts of carbon black N660, 20 parts of nano-inorganic reinforcing agent RC-15, 6.5 parts of oil-naphthenic oil, 0.5 parts of stearic acid 1842 type, 5 parts of C5 resin A-100, 4 parts of tackifying resin SL1802, 9.41 parts of homogenizing agent 40MSF and 0.25 parts of magnesium oxide MAGCHEM 40 were put into an internal mixer with a top bolt pressure of 0.55 MPa, a rotor speed of 30 r / min, a discharge temperature of 125 °C and a mixing time of 160 s to obtain a one-stage mixed rubber; (2) Second stage mixing: put the first stage mixed rubber, 0.5 parts of sulfur powder, 1.5 parts of accelerator MBTS and 1.25 parts of zinc oxide into an internal mixer, with a rotor speed of 25 r / min, a top bolt pressure of 0.55 MPa, a rubber discharge temperature of 107°C and a mixing time of 105 s to obtain the airtight layer rubber.

[0022] Comparative Example 1 A method for preparing an all-steel tire innerliner adhesive comprises the following steps: (1) One-stage mixing: by weight, 77 parts of butyl rubber BIIR-2302, 40 parts of butyl reclaimed rubber, 3 parts of natural rubber, 55 parts of carbon black N660, 6.5 parts of naphthenic oil, 0.5 parts of stearic acid 1842 type, 5 parts of C5 resin A-100, 4 parts of tackifying resin SL1802, 9.41 parts of homogenizer 40MSF and 0.25 parts of magnesium oxide MAGCHEM 40 were put into an internal mixer with a top bolt pressure of 0.55 MPa, a rotor speed of 30 r / min, a discharge temperature of 125 ° C and a mixing time of 160 s to obtain a one-stage mixed rubber; (2) Second stage mixing: put the first stage mixed rubber, 0.5 parts of sulfur powder, 1.5 parts of accelerator MBTS, and 1.25 parts of zinc oxide into an internal mixer with a rotor speed of 25 r / min, a top bolt pressure of 0.55 MPa, a rubber discharge temperature of 107 ° C, and a mixing time of 105 s to obtain the airtight layer rubber.

[0023] The zinc oxide used in Examples 1-5 and Comparative Example 1 is a microcrystalline white powder or white granules obtained from metal by an indirect process, and has a density of 5.55 g / m³.

[0024] Comparison of the physical properties of the all-steel tire innerliner rubber after vulcanization in Examples 1-5 and Comparative Example 1 (vulcanization conditions: 170° C., 20 minutes) is shown in Table 1.

[0025] Table 1 Performance parameters of the all-steel tire innerliner rubber after vulcanization in Examples 1-5 and Comparative Example 1

[0026] The physical property test results shown in Table 1 show that as the amount of nano-inorganic reinforcing agent RC-15 increases, the air permeability coefficient in the test data gradually decreases, indicating that the airtightness of the resulting airtight layer adhesive continues to improve. However, the 300% modulus of elongation first increases and then decreases with the continuous addition of nano-inorganic reinforcing agent RC-15, indicating that the airtight layer adhesive has a certain limit on its load capacity for nano-inorganic reinforcing agent RC-15. The higher the 300% modulus of elongation, the higher the dynamic modulus of the adhesive. This shows that the addition of a certain amount of nano-inorganic reinforcing agent RC-15 to the airtight layer adhesive significantly improves the airtightness and dynamic performance. Moreover, because the addition of nano-inorganic reinforcing agent reduces the adhesive content in the formula, the formulation cost is reduced, which meets the needs of industrialization.

[0027] Finally, it should be noted that the above specific implementation methods are only used to illustrate the technical solutions of the present invention and are not limiting. Although the present invention has been described in detail with reference to examples, those skilled in the art should understand that the technical solutions of the present invention can be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should all be included in the scope of the claims of the present invention.

Claims

1. An all-steel tire inner liner rubber, characterized in that: The invention comprises the following components in parts by weight: 70-85 parts of butyl rubber, 25-45 parts of butyl reclaimed rubber, 3-5 parts of natural rubber, 45-55 parts of carbon black N660, 8-20 parts of nano-inorganic reinforcing agent, 3-8 parts of oil, 0.4-0.6 parts of stearic acid, 4-6 parts of C5 resin, 2-6 parts of tackifying resin, 8-12 parts of homogenizing agent, 0.2-0.4 parts of magnesium oxide, 0.4-0.6 parts of sulfur powder, 1.1-1.6 parts of accelerator and 0.7-1.4 parts of zinc oxide.

2. The all-steel tire inner liner adhesive according to claim 1, characterized in that: The nano inorganic reinforcing agent is a silicate material with a sheet thickness of less than 100nm, a specific surface area of ≥200m² / g, and complies with REACH environmental protection standards.

3. The all-steel tire inner liner adhesive according to claim 1, characterized in that: The oil is environmentally friendly aromatic oil or naphthenic oil.

4. The all-steel tire inner liner adhesive according to claim 1, characterized in that: The C5 resin is hydrogenated C5 petroleum resin.

5. The all-steel tire inner liner adhesive according to claim 1, characterized in that: The tackifying resin is octylphenol formaldehyde tackifying resin.

6. The all-steel tire inner liner adhesive according to claim 1, characterized in that: The butyl rubber includes brominated butyl rubber or chlorinated butyl rubber.

7. The all-steel tire inner liner adhesive according to claim 1, characterized in that: The homogenizer is a hydrocarbon resin mixture 40MSF.

8. The all-steel tire inner liner adhesive according to claim 1, characterized in that: The accelerator is dibenzothiazyl disulfide.

9. The method for preparing the all-steel tire inner liner adhesive according to claim 1, characterized in that: The following steps are involved: (1) One-stage mixing: 70-85 parts of butyl rubber, 25-45 parts of butyl reclaimed rubber, 3-5 parts of natural rubber, 45-55 parts of carbon black N660, 8-20 parts of nano-inorganic reinforcing agent, 3-8 parts of oil, 0.4-0.6 parts of stearic acid, 4-6 parts of C5 resin, 2-6 parts of tackifying resin, 8-12 parts of homogenizer and 0.2-0.4 parts of magnesium oxide are put into an internal mixer, the upper bolt pressure is 0.4-0.59 MPa, the rotor speed is 25-50 r / min, the discharge temperature is 120-140 ° C, and the mixing time is 140-190 s to obtain a one-stage mixed rubber; (2) Second stage mixing: the first stage mixed rubber obtained in step (1), 0.4-0.6 parts of sulfur powder, 1.1-1.6 parts of accelerator and 0.7-1.4 parts of zinc oxide are put into an internal mixer with a rotor speed of 22-30 r / min, a top bolt pressure of 0.4-0.59 MPa, a discharge temperature of 98-110°C and a mixing time of 80-120 s to obtain an airtight layer rubber.