CN115584064A - Variable modulus damping rubber material and preparation method and application thereof - Google Patents
Variable modulus damping rubber material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a variable modulus damping rubber material and a preparation method and application thereof, and belongs to the technical field of engineering structure damping and shock isolation. According to the invention, boric acid modified hydroxyl-terminated polysiloxane is added into a rubber matrix, free radicals are generated under the action of an initiator, and the boric acid modified hydroxyl-terminated polysiloxane is grafted to a molecular chain of the rubber matrix, so that the high elasticity of the rubber material is retained, and simultaneously, the elastic modulus of the rubber material can be subjected to corresponding change under different impact (or shear) speeds, so that the sensitivity of the rubber matrix to the impact speed can be effectively improved, the rubber material can have good seismic reduction and isolation effects under different vibration acceleration conditions, the variability of the rubber matrix modulus is realized, and the elastic modulus range is large.
Description
Technical Field
The invention relates to the technical field of shock absorption and isolation of engineering structures, in particular to a variable modulus shock absorption rubber material and a preparation method and application thereof.
Background
In the field of seismic isolation and reduction of civil engineering, rubber materials are often needed for seismic isolation and reduction, and various energy dissipation elements are combined for energy dissipation so as to reduce the damage of disasters such as earthquake to engineering structures. The elastic modulus of the engineering seismic isolation and reduction rubber material at the present stage is very small in change under different vibration frequencies, and when large vibration is encountered, the modulus of the rubber seismic isolation and reduction element is not enough to resist the vibration, so that the vibration reduction effect is degraded, and the engineering structure is damaged.
Disclosure of Invention
The invention aims to provide a variable modulus damping rubber material, a preparation method and application thereof, which can solve the problems of small elastic modulus range and poor modulus adjustability of rubber materials.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a variable modulus damping rubber material which comprises the following preparation raw materials in parts by weight:
100 parts of a rubber base material, 1 to 3 parts of a coupling agent, 0.3 to 0.6 part of an initiator, 5 to 20 parts of a shear thickening gel, 5 to 10 parts of an active agent, 1 to 4 parts of an anti-aging agent, 40 to 60 parts of carbon black, 1 to 2 parts of a vulcanizing agent and 0 to 3 parts of an accelerator;
the shear thickening gel is boric acid modified hydroxyl-terminated polysiloxane.
Preferably, the rubber substrate comprises a hydrocarbon rubber or a silicone rubber; the hydrocarbon rubber comprises natural rubber, styrene-butadiene rubber, ethylene propylene rubber, butadiene rubber or chloroprene rubber;
the coupling agent comprises a silane coupling agent.
Preferably, the silane coupling agent includes vinyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma- (triethoxysilyl) propyl ] tetrasulfide or vinyltriethoxysilane.
Preferably, the initiator comprises an oxidizing agent and a reducing agent, the oxidizing agent is ammonium persulfate, the reducing agent is sodium bisulfite, and the mass ratio of the oxidizing agent to the reducing agent is 1 (1 to 2).
Preferably, the preparation method of the boric acid modified hydroxyl-terminated polysiloxane comprises the following steps: mixing the a, w-dihydroxy polydimethylsiloxane, boric acid and silicon dioxide, kneading at 140-180 ℃, and dehydrating to obtain boric acid modified hydroxyl-terminated polysiloxane; the mass ratio of the a, w-dihydroxy polydimethylsiloxane, the boric acid and the silicon dioxide is (70-90): 4-10): 5-20).
Preferably, the active agent comprises zinc oxide and stearic acid, and the mass ratio of the zinc oxide to the stearic acid is (2 to 3) to 1;
the anti-aging agent comprises N- (1, 3-dimethyl) butyl-N' -phenyl p-phenylenediamine;
the carbon black is semi-reinforcing carbon black;
the vulcanizing agent comprises sulfur or 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane;
the accelerator comprises a mixture of tetramethylthiuram disulfide and N-cyclohexyl-2-benzothiazole sulfonamide, and the mass ratio of the tetramethylthiuram disulfide to the N-cyclohexyl-2-benzothiazole sulfonamide is (0.2 to 0.4) to 1.
The invention provides a preparation method of the variable modulus damping rubber material, which comprises the following steps:
plasticating a rubber base material, sequentially carrying out first mixing, first rubber discharging and first thin passing on the plasticated rubber base material, an initiator, a coupling agent and shear thickening gel, and grafting the obtained material to obtain a modified base material;
performing second mixing on the modified base material, the active agent, the anti-aging agent and the carbon black, and then performing second rubber discharging and second thin passing in sequence to obtain a section of master batch;
performing third mixing on the primary master batch, the vulcanizing agent and the accelerator, and then sequentially performing third rubber discharging and third thin passing to obtain a mixed rubber;
and vulcanizing the rubber compound to obtain the variable-modulus damping rubber material.
Preferably, the grafting temperature is 60 to 70 ℃, and the time is more than or equal to 8 hours;
the first mixing time is 40 to 60s; the second mixing time is 100 to 140s; the time for the third mixing is 40 to 70s.
Preferably, the number of times of the first thin pass is 3 to 5, and the roll gap is 0.5 to 1mm; the number of times of the second thin pass is 1 to 5, and the roll spacing is 0.5 to 1mm; the number of times of the third thin pass is 2 to 3, and the roll spacing is 0.5 to mm; the vulcanization temperature is 130-180 ℃, the pressure is 5-20MPa, and the time is 20-40min.
The invention provides application of the variable modulus damping rubber material in the technical scheme or the variable modulus damping rubber material prepared by the preparation method in the technical scheme in the field of seismic isolation and reduction in civil engineering.
The invention provides a variable modulus damping rubber material which comprises the following preparation raw materials in parts by weight: 100 parts of a rubber base material, 1 to 3 parts of a coupling agent, 0.3 to 0.6 part of an initiator, 5 to 20 parts of a shear thickening gel, 5 to 10 parts of an active agent, 1 to 4 parts of an anti-aging agent, 40 to 60 parts of carbon black, 1 to 2 parts of a vulcanizing agent and 0 to 3 parts of an accelerator; the shear thickening gel is boric acid modified hydroxyl-terminated polysiloxane. The shear thickening gel adopted by the invention is boric acid modified hydroxyl-terminated polysiloxane, the boric acid modified hydroxyl-terminated polysiloxane is in a viscous flow state under quasi-static load and is in a solid state under dynamic load, and the modulus of the material is greatly improved in the process of converting from a viscous flow state to a solid state, so that the boric acid modified hydroxyl-terminated polysiloxane can absorb and dissipate a part of energy through the rapid change of the viscosity when being impacted, sheared and the like. According to the invention, boric acid modified hydroxyl-terminated polysiloxane is added into a rubber matrix, free radicals are generated under the action of an initiator, and the boric acid modified hydroxyl-terminated polysiloxane is grafted onto a molecular chain of the rubber matrix, so that the high elasticity of the rubber material is retained, and meanwhile, the rubber material is endowed with the performance that the elastic modulus can be subjected to corresponding change under different impact (or shearing) speeds, so that the sensitivity of the rubber matrix to the impact speed can be effectively improved, the rubber material can have good seismic isolation and reduction effects under different vibration acceleration conditions, the variability of the rubber matrix modulus is realized, the elastic modulus range is large, and the elastic modulus can be increased by 2 times along with the acceleration of the impact (or shearing) speed.
The elastic modulus of the variable modulus shock absorption rubber material provided by the invention is improved along with the increase of the impact velocity, the elastic modulus and the impact velocity form a nonlinear relation (the elastic modulus of the existing rubber material is slightly changed and is not obviously changed along with the change of the impact velocity), and when strong shock occurs, the elastic modulus of the rubber material can be greatly improved, the deformation of shock absorption and isolation elements is reduced, the structural damage of buildings is avoided, and the variable modulus shock absorption rubber material has important significance in the field of shock absorption and isolation of civil engineering.
Drawings
FIG. 1 is a shear rate-shear modulus graph of rubber materials of examples 1 to 5 and comparative example 1;
FIG. 2 shows the proof of purchase of the shear thickening gels used in examples 1 to 5.
Detailed Description
The invention provides a variable modulus damping rubber material which comprises the following preparation raw materials in parts by weight:
100 parts of a rubber base material, 1 to 3 parts of a coupling agent, 0.3 to 0.6 part of an initiator, 5 to 20 parts of a shear thickening gel, 5 to 10 parts of an active agent, 1 to 4 parts of an anti-aging agent, 40 to 60 parts of carbon black, 1 to 2 parts of a vulcanizing agent and 0 to 3 parts of an accelerator;
the shear thickening gel is boric acid modified hydroxyl-terminated polysiloxane.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
The variable modulus damping rubber material comprises 100 parts by weight of rubber base material, wherein the rubber base material preferably comprises hydrocarbon rubber or silicon rubber; the hydrocarbon rubber preferably comprises natural rubber, styrene-butadiene rubber, ethylene-propylene rubber, butadiene rubber or chloroprene rubber. The olefin rubber used in the invention has good elasticity and higher mechanical property.
On the basis of the weight parts of the rubber base material, the raw materials for preparing the variable modulus damping rubber material comprise 1 to 3 parts of coupling agent, preferably 2 to 2.5 parts; the coupling agent preferably includes a silane-based coupling agent, which preferably includes vinyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma- (triethoxysilyl) propyl ] tetrasulfide, or vinyltriethoxysilane. The invention effectively improves the grafting rate of the shear thickening gel on the rubber matrix by utilizing the modification effect of the coupling agent.
The preparation raw materials of the variable modulus damping rubber material provided by the invention comprise 0.3 to 0.6 part of initiator by weight based on the weight parts of the rubber base material, the initiator preferably comprises oxidant and reductant, the oxidant is preferably ammonium persulfate, the reductant is preferably sodium bisulfite, and the mass ratio of the oxidant to the reductant is preferably 1 (1 to 2), and more preferably 1. The invention leads the shear thickening gel to react to generate free radicals under the action of a reducing agent, and the free radicals are grafted to the molecular chain of the rubber matrix under the action of an oxidizing agent.
On the basis of the weight parts of the rubber base material, the raw materials for preparing the variable modulus damping rubber material provided by the invention comprise 5 to 20 parts of shear thickening gel, preferably 8 to 15 parts; the shear thickening gel is boric acid modified hydroxyl-terminated polysiloxane (a daub-state silicon polymer material with a shear thickening effect).
In the present invention, the method for preparing the boric acid-modified hydroxyl-terminated polysiloxane preferably comprises: mixing the a, w-dihydroxy polydimethylsiloxane, boric acid and silicon dioxide, kneading at 140-180 ℃, and dehydrating to obtain the boric acid modified hydroxyl-terminated polysiloxane. In the invention, the mass ratio of the a, the w-dihydroxy polydimethylsiloxane, the boric acid and the silicon dioxide is preferably (70 to 90): (4 to 10): 5 to 20).
The mixing of the a, w-dihydroxy polydimethylsiloxane, the boric acid and the silicon dioxide is not particularly limited in the invention, and the materials are uniformly mixed according to the well-known process in the field. In the present invention, the kneading temperature is preferably 140 to 180 ℃; the specific operation of the kneading and dehydrating in the present invention is not particularly limited, and may be carried out according to a procedure well known in the art.
The preparation raw material of the variable modulus damping rubber material comprises 5 to 10 parts of an active agent, preferably 6 to 9 parts, and more preferably 7 to 8 parts by weight of the rubber base material; in the invention, the active agent preferably comprises zinc oxide and stearic acid, and the mass ratio of the zinc oxide to the stearic acid is preferably (2 to 3): 1, and more preferably 2.5. The invention utilizes the activator to activate the vulcanization system consisting of the accelerator and the vulcanizing agent in the vulcanization process, improves the crosslinking density and the heat resistance of the rubber material, and can effectively improve the mechanical property and the elasticity of the rubber material.
Based on the weight parts of the rubber base material, the raw material for preparing the variable modulus damping rubber material comprises 1 to 4 parts of an anti-aging agent, preferably 2 to 3 parts; the anti-aging agent preferably comprises N- (1, 3-dimethyl) butyl-N' -phenyl-p-phenylenediamine. The invention improves the aging resistance of the rubber material by adding the anti-aging agent and prolongs the service life of the rubber material.
On the basis of the weight parts of the rubber base material, the raw material for preparing the variable modulus damping rubber material comprises 40 to 60 parts of carbon black, preferably 45 to 55 parts, and more preferably 50 parts; the carbon black is preferably a semi-reinforcing carbon black; the semi-reinforcing carbon black is preferably carbon black N774 or carbon black N762. The invention improves the mechanical property of the rubber material through the reinforcing effect of the carbon black, and endows the rubber material with higher strength and elongation.
On the basis of the weight parts of the rubber base material, the raw materials for preparing the variable modulus damping rubber material provided by the invention comprise 1 to 2 parts of vulcanizing agent, preferably 1.3 to 1.6 parts, and more preferably 1.5 parts; the vulcanizing agent preferably includes sulfur or 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane.
The raw materials for preparing the variable modulus damping rubber material comprise 0 to 3 parts of accelerator, preferably 1.2 to 1.7 parts, and more preferably 1.4 parts by weight of the rubber base material. In the present invention, the accelerator preferably comprises a mixture of tetramethylthiuram disulfide (TMTD) and N-cyclohexyl-2-benzothiazolesulfenamide (CZ), the mass ratio of tetramethylthiuram disulfide and N-cyclohexyl-2-benzothiazolesulfenamide being preferably (0.2 to 0.4): 1, more preferably 0.33. When the rubber substrate is a silicone rubber, an accelerator is not required. Under the action of a vulcanizing agent and an accelerator, the rubber material has a three-dimensional network formed by rubber molecular chains, has good elasticity, can adapt to various large deformations, and has good shock absorption and isolation performance.
The invention provides a preparation method of the variable modulus damping rubber material, which comprises the following steps:
plasticating a rubber base material, sequentially carrying out first mixing, first glue discharging and first thin passing on the plasticated rubber base material, an initiator, a coupling agent and shear thickening gel, and grafting the obtained material to obtain a modified base material;
carrying out second mixing on the modified base material, the activating agent, the anti-aging agent and the carbon black, and then sequentially carrying out second rubber discharging and second thin passing to obtain a section of master batch;
performing third mixing on the first-stage master batch, the vulcanizing agent and the accelerator, and then sequentially performing third rubber discharging and third thin passing to obtain a mixed rubber;
and vulcanizing the rubber compound to obtain the variable modulus damping rubber material.
According to the invention, after a rubber base material is plasticated, the plasticated rubber base material, an initiator, a coupling agent and shear thickening gel are sequentially subjected to first mixing, first rubber discharging and first thin passing, and the obtained material is grafted to obtain a modified base material.
The invention preferably plasticates to 120 ℃ in an internal mixer; and then adding the initiator, the coupling agent and the shear thickening gel into an internal mixer to perform first mixing, first rubber discharging and first thin passing.
In the invention, the time for the first mixing is preferably 40 to 60s, and more preferably 50 to 55s; the conditions of the first stripping are not particularly limited in the present invention, and the first stripping may be performed according to a process well known in the art.
The invention preferably performs the first thin pass on an open mill; the number of the first thin pass is preferably 3 to 5, and more preferably 4; the roll gap is preferably 0.5 to 1mm, more preferably 0.6 to 0.9mm, and still more preferably 0.7 to 0.8mm.
In the invention, the grafting temperature is preferably 60 to 70 ℃, and the time is preferably not less than 8h; the invention preferably takes the material after rubber discharge out of the internal mixer, and stands for more than or equal to 8 hours to realize grafting; in the grafting process, the shear thickening gel is grafted to the rubber substrate, so that the shear thickening gel modifies the rubber substrate.
After the modified base material is obtained, the modified base material, the activating agent, the anti-aging agent and the carbon black are subjected to secondary mixing, and then secondary rubber discharging and secondary thin passing are sequentially performed to obtain a section of master batch.
In the present invention, the second mixing preferably includes a first mixing and a second mixing performed in this order, and the time for the second mixing is preferably 100 to 140s. In the invention, the modified base material is preferably put into an internal mixer again, the active agent and the anti-aging agent are sequentially added, the mixture is subjected to primary mixing for 40 to 60s (more preferably 50 s), carbon black is added, and the mixture is subjected to secondary mixing for 60 to 80s (more preferably 70 s), and then secondary rubber discharge is performed. The second glue removal is not particularly limited in the present invention, and may be performed according to a process well known in the art.
In the invention, the second thin pass is preferably carried out on an open mill, the number of times of the second thin pass is preferably 1 to 5, and the roll gap is preferably 0.5 to 1mm, and more preferably 0.7 to 0.8mm.
After the second thin-pass is finished, the obtained primary rubber is preferably taken out of the internal mixer and is parked for more than or equal to 8 hours at normal temperature.
After the first-section master batch is obtained, the first-section master batch, the vulcanizing agent and the accelerator are subjected to third mixing, and then third rubber discharging and third thin passing are sequentially performed to obtain the mixed rubber.
Preferably, the first-stage master batch is put into an internal mixer, and a vulcanizing agent and an accelerator are added to carry out third mixing and third rubber discharge; the time for the third mixing is preferably 40 to 70s, and more preferably 50 to 60s; the third glue-discharging is not particularly limited in the present invention, and may be performed according to a process well known in the art.
The invention preferably carries out the third thin pass on the open mill; the number of the third thin pass is preferably 2 to 3, and more preferably 2; the roll gap is preferably 0.5 to 1mm, and more preferably 0.6 to 0.8mm; after the third thin pass is completed, the obtained rubber material is preferably parked for 8 hours to obtain a rubber compound.
After the rubber compound is obtained, the rubber compound is vulcanized to obtain the variable modulus damping rubber material.
In the invention, the temperature of vulcanization is preferably 130 to 180 ℃, more preferably 135 to 150 ℃, and further preferably 140 to 145 ℃; the pressure is preferably 5 to 20MPa, more preferably 12 to 18MPa, and still more preferably 14 to 15MPa; the time is preferably 20 to 40min, and more preferably 25 to 30min; the vulcanization is preferably carried out in a press vulcanizer; the press vulcanizer of the present invention is not particularly limited, and may be a corresponding apparatus known in the art.
The invention provides application of the variable modulus damping rubber material in the technical scheme or the variable modulus damping rubber material prepared by the preparation method in the technical scheme in the field of seismic isolation and reduction in civil engineering. The method of the present invention is not particularly limited, and the method may be applied according to a method known in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all 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.
In the following examples, the shear thickening gel-boric acid modified hydroxy terminated polysiloxane model was purchased from sienpike xuanfu new materials ltd, see fig. 2;
the anti-aging agent is N- (1, 3-dimethyl) butyl-N' -phenyl-p-phenylenediamine.
Example 1
adding 0.1 part by weight of ammonium persulfate, 0.2 part by weight of sodium bisulfite, 1 part by weight of coupling agent (vinyl trimethoxy silane) and 5 parts by weight of shear thickening gel into an internal mixer, mixing for 50 seconds, then discharging rubber, thinly passing on an open mill for 4 times with the roll spacing of 0.7mm, and standing for 8 hours under the environment of 60 to 70 ℃;
putting the parked natural rubber into an internal mixer again, sequentially adding 4 parts by weight of zinc oxide, 2 parts by weight of stearic acid and 2 parts by weight of an anti-aging agent, mixing for 50 seconds, adding 45 parts by weight of carbon black N774, mixing for 60 seconds, discharging rubber, thinly passing through an open mill for 3 times with the roller spacing of 0.5mm to prepare a section of master batch, and parking for 8 hours at normal temperature;
putting the first-section master batch into an internal mixer, sequentially adding 1.5 parts by weight of sulfur as a vulcanizing agent, 1.0 part by weight of CZ and 0.2 part by weight of TMTD, mixing for 50 seconds to discharge rubber, thinly passing the mixture on an open mill for 2 times with the roller spacing of 0.6mm, and standing the rubber for 8 hours to obtain rubber compound;
and (3) putting the rubber compound into a mold, and vulcanizing in a flat vulcanizing machine at the vulcanization temperature of 135 ℃, under the pressure of 12MPa for 40 minutes to obtain the rubber material.
Example 2
adding 0.2 part by weight of ammonium persulfate, 0.2 part by weight of sodium bisulfite, 2 parts by weight of coupling agent (gamma-methacryloxypropyltrimethoxysilane) and 8 parts by weight of shear thickening gel into an internal mixer, mixing for 55 seconds, then discharging rubber, thinly passing on an open mill for 4 times with the roller spacing of 0.6mm, and standing for 8 hours at the temperature of 60-70 ℃;
putting the parked styrene butadiene rubber into an internal mixer again, sequentially adding 5 parts by weight of zinc oxide, 2 parts by weight of stearic acid and 3 parts by weight of an anti-aging agent, mixing for 50 seconds, adding 50 parts by weight of carbon black N774, mixing for 70 seconds, discharging rubber, thinly passing through an open mill for 2 times with the roll spacing of 0.8mm to prepare a section of master batch, and standing at normal temperature for 8 hours;
putting the first-section master batch into an internal mixer, sequentially adding 1.3 parts by weight of vulcanizing agent (sulfur), 0.9 part by weight of accelerator CZ and 0.3 part by weight of accelerator TMTD, mixing for 60 seconds to discharge rubber, thinly passing through an open mill for 3 times with the roller spacing of 0.8mm, and standing the rubber for 8 hours to obtain rubber compound;
and putting the rubber compound into a mold, and vulcanizing in a flat vulcanizing machine at the vulcanization temperature of 140 ℃, under the pressure of 14MPa for 30 minutes to obtain the rubber material.
Example 3
adding 0.2 part by weight of ammonium persulfate, 0.4 part by weight of sodium bisulfite, 3 parts by weight of coupling agent (gamma- (triethoxysilyl) propyl ] tetrasulfide) and 15 parts by weight of shear thickening gel into an internal mixer, mixing for 50 seconds, then discharging rubber, thinly passing on an open mill for 5 times with the roller distance of 0.8mm, and standing for 8 hours at the temperature of 60-70 ℃;
putting the parked ethylene propylene diene monomer rubber into an internal mixer again, sequentially adding 5 parts by weight of zinc oxide, 2.5 parts by weight of stearic acid and 2 parts by weight of an anti-aging agent, mixing for 50 seconds, adding 60 parts by weight of carbon black N762, mixing for 70 seconds, discharging rubber, thinly passing through an open mill for 3 times with the roller spacing of 0.5mm to prepare a section of masterbatch, and standing at normal temperature for 8 hours;
putting a section of master batch into an internal mixer, sequentially adding 1.6 parts by weight of sulfur as a vulcanizing agent, 1.2 parts by weight of CZ and 0.4 part by weight of TMTD, mixing for 60 seconds to discharge rubber, thinly passing the mixture on an open mill for 3 times with the roller spacing of 0.5mm, and standing the rubber material for 8 hours at normal temperature to obtain rubber compound;
and putting the prepared rubber compound into a mold, and vulcanizing in a flat vulcanizing machine at the vulcanization temperature of 143 ℃, the pressure of 15MPa and the time of 30 minutes to obtain the rubber material.
Example 4
adding 0.25 weight part of ammonium persulfate, 0.3 weight part of sodium bisulfite, 2.5 weight parts of coupling agent (vinyl triethoxysilane) and 20 weight parts of shear thickening gel into an internal mixer, mixing for 60 seconds, then discharging rubber, thinly passing through an open mill for 4 times with the roller spacing of 1mm, and standing for 8 hours at the temperature of 60-70 ℃;
putting the parked silicone rubber into an internal mixer again, adding 3.5 parts by weight of zinc oxide, 1.5 parts by weight of stearic acid and 1 part by weight of an anti-aging agent in sequence, mixing for 50 seconds, adding 55 parts by weight of carbon black N762, mixing for 70 seconds, discharging rubber, thinly passing through an open mill for 1 time with the roller spacing of 1mm to prepare a section of master batch, and parking for 8 hours at normal temperature;
putting the first-stage master batch into an internal mixer, sequentially adding 2.0 parts by weight of vulcanizing agent 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane, mixing for 60 seconds to remove rubber, thinly passing on an open mill for 2 times with the roller spacing of 0.8mm, and standing the rubber for 8 hours at normal temperature to obtain rubber compound;
and putting the rubber compound into a mold, and vulcanizing in a flat vulcanizing machine at the vulcanization temperature of 145 ℃, under the pressure of 17MPa for 25 minutes to obtain the rubber material.
Example 5
adding 0.3 part by weight of ammonium persulfate, 0.3 part by weight of sodium bisulfite, 3 parts by weight of coupling agent vinyltriethoxysilane and 12 parts by weight of shear thickening gel into an internal mixer, mixing for 60 seconds, discharging rubber, passing through an open mill for 3 times with a roll gap of 0.9mm, and standing for 8 hours at the temperature of 60-70 ℃;
putting the parked chloroprene rubber into an internal mixer again, sequentially adding 5 parts by weight of zinc oxide, 2.5 parts by weight of stearic acid and 4 parts by weight of anti-aging agent, mixing for 50 seconds, adding 50 parts by weight of carbon black N774, mixing for 70 seconds, discharging rubber, thinly passing on an open mill for 2 times with the roller spacing of 0.7mm to prepare a section of masterbatch, and standing at normal temperature for 8 hours;
putting a section of master batch into an internal mixer, sequentially adding 1.5 parts by weight of sulfur as a vulcanizing agent, 1.0 part by weight of CZ and 0.4 part by weight of TMTD, mixing for 50 seconds to discharge rubber, thinly passing the mixture on an open mill for 3 times with the roller spacing of 0.6mm, and standing the rubber material for 8 hours at normal temperature to obtain rubber compound;
and putting the rubber compound into a mold, and vulcanizing in a flat vulcanizing machine at the vulcanization temperature of 150 ℃, under the pressure of 18MPa for 20 minutes to obtain the rubber material.
Comparative example 1
standing at room temperature for 13 hours, adding 1.6 parts by weight of sulfur, 1.3 parts by weight of benzothiazole disulfide and 1.1 part by weight of N-cyclohexyl-2-benzothiazole sulfonamide into an internal mixer, and uniformly mixing to obtain a rubber compound;
and putting the rubber compound into a mold, and vulcanizing in a flat vulcanizing machine at the vulcanizing temperature of 140 ℃, under the pressure of 8MPa for 15 minutes to obtain the rubber material.
Performance detection
The performance of the rubber material is tested according to the method recorded in GB/T9870.1-2006 determination of dynamic performance of vulcanized rubber or thermoplastic rubber, the rubber test piece adopts a two-piece shear mode, the performance parameter shear modulus can be obtained, the product modulus is calculated according to the shear modulus and the product structure, and the obtained result is shown in Table 1.
TABLE 1 Performance data of the rubber materials of examples 1 to 5 and comparative example 1
As can be seen from the data in Table 1, the shear modulus of the rubber material provided by the invention is gradually increased along with the increase of the shear speed, and the maximum increase can reach 195%, while the shear modulus of the traditional rubber material in the comparative example 1 is not obviously changed along with the increase of the shear speed and is only 24.7%, which shows that the variable modulus damping rubber material provided by the invention can realize better modulus correspondence under different vibrations and is suitable for vibration damping of different grades.
FIG. 1 is a shear rate-shear modulus curve diagram of rubber materials of examples 1 to 5 and comparative example 1, and it can be seen from FIG. 1 that the shear modulus increase rate of the rubber materials provided in examples 1 to 5 shows a nonlinear increase with the increase of the shear rate, which shows that the higher the shear rate is, the higher the shear modulus increase rate is; whereas the rubber material of comparative example 1 does not have a non-linear relationship.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The variable modulus damping rubber material is characterized by comprising the following preparation raw materials in parts by weight:
100 parts of a rubber base material, 1 to 3 parts of a coupling agent, 0.3 to 0.6 part of an initiator, 5 to 20 parts of a shear thickening gel, 5 to 10 parts of an active agent, 1 to 4 parts of an anti-aging agent, 40 to 60 parts of carbon black, 1 to 2 parts of a vulcanizing agent and 0 to 3 parts of an accelerator;
the shear thickening gel is boric acid modified hydroxyl-terminated polysiloxane;
the preparation method of the boric acid modified hydroxyl-terminated polysiloxane comprises the following steps: mixing alpha, omega-dihydroxy polydimethylsiloxane, boric acid and silicon dioxide, kneading at 140-180 ℃, and dehydrating to obtain boric acid modified hydroxyl-terminated polysiloxane;
the initiator comprises an oxidizing agent and a reducing agent, wherein the oxidizing agent is ammonium persulfate, and the reducing agent is sodium bisulfite.
2. A variable modulus shock absorbing rubber material as claimed in claim 1, wherein said rubber substrate comprises hydrocarbon rubber or silicone rubber; the hydrocarbon rubber comprises natural rubber, styrene-butadiene rubber, ethylene propylene rubber, butadiene rubber or chloroprene rubber;
the coupling agent comprises a silane coupling agent.
3. A shock absorbing rubber material with variable modulus as claimed in claim 2, wherein said silane coupling agent comprises vinyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma- (triethoxysilyl) propyl tetrasulfide or vinyltriethoxysilane.
4. The variable modulus damping rubber material as claimed in claim 1, wherein the mass ratio of the oxidant to the reducing agent is 1 (1-2).
5. The variable modulus damping rubber material as claimed in claim 1, wherein the mass ratio of the alpha, omega-dihydroxy polydimethylsiloxane to the boric acid to the silicon dioxide is (70-90): (4-10): and (5-20).
6. The variable modulus damping rubber material as claimed in claim 1, wherein the active agent comprises zinc oxide and stearic acid, and the mass ratio of the zinc oxide to the stearic acid is (2 to 3): 1;
the anti-aging agent comprises N- (1, 3-dimethyl) butyl-N' -phenyl p-phenylenediamine;
the carbon black is semi-reinforcing carbon black;
the vulcanizing agent comprises sulfur or 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane;
the accelerator comprises a mixture of tetramethylthiuram disulfide and N-cyclohexyl-2-benzothiazole sulfonamide, wherein the mass ratio of the tetramethylthiuram disulfide to the N-cyclohexyl-2-benzothiazole sulfonamide is (0.2 to 0.4) to 1.
7. The preparation method of the variable modulus damping rubber material of any one of claims 1 to 6, characterized by comprising the following steps:
plasticating a rubber base material, sequentially carrying out first mixing, first rubber discharging and first thin passing on the plasticated rubber base material, an initiator, a coupling agent and shear thickening gel, and grafting the obtained material to obtain a modified base material;
carrying out second mixing on the modified base material, the activating agent, the anti-aging agent and the carbon black, and then sequentially carrying out second rubber discharging and second thin passing to obtain a section of master batch;
performing third mixing on the first-stage master batch, the vulcanizing agent and the accelerator, and then sequentially performing third rubber discharging and third thin passing to obtain a mixed rubber;
and vulcanizing the rubber compound to obtain the variable modulus damping rubber material.
8. The preparation method of claim 7, wherein the grafting temperature is 60 to 70 ℃, and the grafting time is not less than 8h;
the first mixing time is 40 to 60s; the second mixing time is 100 to 140s; the time for the third mixing is 40 to 70s.
9. The preparation method according to claim 7, wherein the number of the first thin passes is 3 to 5, and the roll gap is 0.5 to 1mm; the number of times of the second thin pass is 1 to 5, and the roll spacing is 0.5 to 1mm; the number of times of the third thin pass is 2 to 3, and the roll spacing is 0.5 to mm; the vulcanization temperature is 130 to 180 ℃, the pressure is 5 to 20MPa, and the time is 20 to 40min.
10. The application of the shock absorption rubber material with variable modulus as defined in any one of claims 1 to 6 or the shock absorption rubber material with variable modulus prepared by the preparation method as defined in any one of claims 7 to 9 in the seismic isolation and reduction field of civil engineering.
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| CN117801392A (en) * | 2024-03-01 | 2024-04-02 | 中裕铁信交通科技股份有限公司 | Rubber shock pad for tunnel lining and preparation method and application thereof |
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