CN103146322A - Reclaimed butyl rubber damping adhesive - Google Patents

Reclaimed butyl rubber damping adhesive Download PDF

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Publication number
CN103146322A
CN103146322A CN2013100702866A CN201310070286A CN103146322A CN 103146322 A CN103146322 A CN 103146322A CN 2013100702866 A CN2013100702866 A CN 2013100702866A CN 201310070286 A CN201310070286 A CN 201310070286A CN 103146322 A CN103146322 A CN 103146322A
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damping
test
temperature
reclaimed rubber
rubber
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CN2013100702866A
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吴驰飞
卫艳玲
吴登杰
许海燕
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East China University of Science and Technology
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East China University of Science and Technology
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Priority to CN2013100702866A priority Critical patent/CN103146322A/en
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Abstract

The invention relates to a reclaimed butyl rubber damping adhesive. The reclaimed butyl rubber damping adhesive is characterized in that the damping adhesive is prepared by mixing and preforming the following raw materials in parts by weight: 50-100 parts of reclaimed butyl rubber, 0-100 parts of butyl rubber, 50-250 parts of a damping endowing agent, and 100-800 parts of inorganic filler. According to the reclaimed butyl rubber damping adhesive prepared, the damping property of the butyl rubber can be obviously improved, the material has good adhesive property and has the properties of damping materials and adhesives.

Description

A kind of butyl reclaimed rubber is the damping sizing agent
Technical field
The present invention relates to butyl reclaimed rubber series high-performance damping gluing agent material formula, particularly take butyl reclaimed rubber as matrix, the high performance material take damping imparting agent and mineral filler as additive.
Background technology
High polymer damping material is based on the visco-elasticity of superpolymer, and namely in the glass transition zone, the internal friction that is produced by molecular chain movement partly changes mechanical energy or the acoustic energy of outer field action into heat energy dissipation, and has the functional materials of damping noise reduction effect.In addition, the distinctive viscoelasticity behavior of macromolecular material makes colloid under less power effect, viscous fluid flow occur, and and formed Van der Waals force between glutinous thing, thereby produce higher bonding force, make it be used to sizing agent.
The temperature range of the glass transition of general homopolymer is narrow, and the temperature range that produces effective damping is roughly near second-order transition temperature ± and 10~15 ℃, the use temperature of material is limited in scope.The glass transition region. of rubber type of material occurs in below room temperature mostly, can not well satisfy the actual needs that use.Therefore, development use temperature a wider range and controlled damping material become this area technical problem in the urgent need to address.
Isoprene-isobutylene rubber is the multipolymer of polybutene and a small amount of polyisoprene, in its molecular structure, the methyl of a large amount of regular arrangements makes isoprene-isobutylene rubber have the advantages such as low air penetrability, Heat stability is good, damping performance are good, anti-ozone, is widely used in the fields such as aerospace cause, communications and transportation, mechanical means, construction work and daily life.Yet isoprene-isobutylene rubber due to self curability and self-adhesion not good enough, therefore make its application in the sizing agent field only limit to insulating glass sealant, the industry such as automobile sealed.
Along with a large amount of uses of isoprene-isobutylene rubber, the quantity of waste butyl rubber is also increasing.Reclaimed rubber is main path and the method that waste butyl rubber is recycled, and it is the rubber that has certain plasticity-and can again vulcanize, and with itself and rubber and use, can save rubber, and reduction power consumption of polymer processing and product cost are improved processing performance.And the butyl reclaimed rubber good processability, the very fast and operational safety of vulcanization rate generally can incipient scorch, is easy to mixing, calendering, and power consumption is few.
Butyl reclaimed rubber series high-performance damping gluing agent material has the damping capacity that is better than isoprene-isobutylene rubber, and has overcome the not good enough shortcoming of isoprene-isobutylene rubber material self-adhesion, has good damping capacity and adhesive property, is a kind of high performance damping sizing agent.
Summary of the invention
The object of the invention is, a kind of high damping properties material with wide use temperature scope is provided, and this material has the sizing agent performance simultaneously.
The present invention adds organic low-molecular weight compound and mineral filler in macromolecular compound, form a kind of homodisperse molecular complex.Utilize polymer and low molecular interaction to present high damping characteristic, widen simultaneously the use temperature scope of damping material and make damping material have good adhesive property.
The present invention is realized by following technical scheme:
A kind of butyl reclaimed rubber is the damping sizing agent, it is characterized in that, said damping sizing agent prepares by the following method: 1) feed composition and ratio of quality and the number of copies are:
Butyl reclaimed rubber: 50-100 part
Isoprene-isobutylene rubber: 0-100 part
Damping imparting agent: 50-250 part
Mineral filler: 100-800 part
The mooney viscosity ML[(1+4 of described butyl reclaimed rubber) 100 ℃] be 5-60,
Described damping imparting agent is petroleum resin or rosin,
Described mineral filler is barium sulfate or calcium carbonate,
2) add the Haake torque rheometer mixing described raw material in described ratio, temperature is 20-120 ℃, and the time is 10-30min, after mixing, and compressing tablet on vulcanizing press, making described butyl reclaimed rubber is the damping sizing agent.
The present invention adopts dynamic mechanical analyzer (DMA) to carry out the dynamic mechanical test analysis to damping material.Test condition: frequency 11Hz, temperature-60-120 ℃, 3 ℃/min of temperature rise rate adopts stretching clamp.
Adopt rotational viscosimeter to be rotated viscosity test to material.Testing method is tested according to GB GB/T2794-1995.
Adopt softening point apparatus material to be carried out the test of softening temperature.Testing method is tested according to GB GB/T15332-94.
Adopt omnipotent test drawing machine to carry out 180 ° of peel strength tests to material.180 ° of peel strength test methods are tested according to GB/T2790-1995.
Beneficial effect
The prepared butyl reclaimed rubber of the present invention is the damping capacity that the damping sizing agent can significantly improve isoprene-isobutylene rubber, and makes material have good adhesive property, has had the performance of damping material and sizing agent concurrently, makes simultaneously its performance be better than the isoprene-isobutylene rubber material.
Description of drawings
Fig. 1 is that isoprene-isobutylene rubber/butyl reclaimed rubber (A)/petroleum resin=50/50/180 dynamic mechanical test is analyzed collection of illustrative plates.
Fig. 2 is butyl reclaimed rubber (A)/petroleum resin/barium sulfate=100/180/300 dynamic mechanical analysis collection of illustrative plates.
Fig. 3 is butyl reclaimed rubber (A)/petroleum resin/calcium carbonate=100/180/300 dynamic mechanical analysis collection of illustrative plates.
Fig. 4 is butyl reclaimed rubber (A)/rosin/barium sulfate=100/180/300 dynamic mechanical collection of illustrative plates.
Fig. 5 is butyl reclaimed rubber (A)/rosin/barium sulfate=100/180/800 dynamic mechanical collection of illustrative plates.
Fig. 6 is butyl reclaimed rubber (B)/rosin/barium sulfate=100/180/800 dynamic mechanical collection of illustrative plates.
Fig. 7 is that isoprene-isobutylene rubber/petroleum resin=100/180/300 dynamic mechanical test is analyzed collection of illustrative plates
Fig. 8 is isoprene-isobutylene rubber/rosin/barium sulfate=100/180/800 dynamic mechanical collection of illustrative plates.
Embodiment
Content of the present invention is further elaborated by following embodiment and accompanying drawing, but does not limit the scope of the invention.
As follows with the physical significance of dynamic mechanical analyzer DMA relevant parameters:
tanδ=E’’/E’
Tan δ-----dissipation factor
E ' '-----out-of-phase modulus
E '-----storage modulus
Embodiment 1:50 gram butyl reclaimed rubber (A) and 50 gram isoprene-isobutylene rubbers join in the Haake torque rheometer, then add 180 gram petroleum resin and 300 gram barium sulfate, after mixing, adopt vulcanizing press to prepare 2mm slab-like material sample.Adopt dynamic mechanical analyzer (DMA) to carry out dynamic mechanical test to it.Test condition: frequency 11Hz, temperature--60~120 ℃, 3 ℃/min of temperature rise rate adopts stretching clamp, and test result is seen Fig. 1.As seen from Figure 1, the damping factor peak value of this material is 3.02, and peak value is positioned at 25.8 ℃.
Embodiment 2:100 gram butyl reclaimed rubber (A) joins in the Haake rheometer, then adds 180 gram petroleum resin and 300 gram barium sulfate, after mixing, adopts vulcanizing press to prepare 2mm slab-like material sample.Adopt dynamic mechanical analyzer (DMA) to carry out dynamic mechanical test to it.Test condition: frequency 11Hz, temperature--60~120 ℃, 3 ℃/min of temperature rise rate adopts stretching clamp, and test result is seen Fig. 2.As seen from Figure 2, the damping factor peak value of this material is 4.46, and peak value is positioned at 24.9 ℃.
Embodiment 3:100 gram butyl reclaimed rubber (A) joins in the Haake rheometer, then adds 180 gram petroleum resin and 300 gram calcium carbonate, after mixing, adopts vulcanizing press to prepare 2mm slab-like material sample.Adopt dynamic mechanical analyzer (DMA) to carry out dynamic mechanical test to it.Test condition: frequency 11Hz, temperature--60~120 ℃, 3 ℃/min of temperature rise rate adopts stretching clamp, and test result is seen Fig. 3.As seen from Figure 3, the damping factor peak value of this material is 4.12, and peak value is positioned at 24.8 ℃.
Embodiment 4:100 gram butyl reclaimed rubber (A) joins in the Haake rheometer, then adds 180 gram rosin and 300 gram barium sulfate, after mixing, adopts vulcanizing press to prepare 2mm slab-like material sample.Adopt dynamic mechanical analyzer (DMA) to carry out dynamic mechanical test to it.Test condition: frequency 11Hz, temperature--60~120 ℃, 3 ℃/min of temperature rise rate adopts stretching clamp, and test result is seen Fig. 4.As seen from Figure 4, the damping factor peak value of this material is 3.98, and peak value is positioned at 23.8 ℃.Dissipation factor is 5.8-63.9 ℃ greater than 1 temperature range, at the temperature range internal loss factors of-3.2 ℃ to 100 ℃ all greater than 0.5.
Embodiment 5:100 gram butyl reclaimed rubber (A) joins in the Haake rheometer, then adds 180 gram rosin and 800 gram barium sulfate, after mixing, adopts vulcanizing press to prepare 2mm slab-like material sample.Adopt dynamic mechanical analyzer (DMA) to carry out dynamic mechanical test to it.Test condition: frequency 11Hz, temperature--60~120 ℃, 3 ℃/min of temperature rise rate adopts stretching clamp, and test result is seen Fig. 5.As seen from Figure 5, the damping factor peak value of this material is 4.01, and peak value is positioned at 25.8 ℃.Dissipation factor is 8.9-64.8 ℃ greater than 1 temperature range, at the temperature range internal loss factor of 0.8 ℃ to 102 ℃ all greater than 0.5.
Adopt rotational viscosimeter to carry out the viscosity test to it, during mensuration, the instrument level is arranged on fixed support, then look the viscosity size, select suitable rotor and rotating speed, make reading at the 15%-85% of scale card, probe temperature is 180 ℃, and test result sees Table 1.As can be seen from Table 1, this material is 8749mPas at the rotation viscosity of 180 ℃.Adopt softening point apparatus to carry out the softening temperature test to material, test result sees Table 1, and as shown in Table 1, the softening temperature of this material is 81.5 ℃.
Adopt omnipotent test drawing machine to carry out mechanical test to it.Initial bonding strength is tested according to GB/T2790-1995.Sample is placed in 80 ℃ of constant temperature 336h, the cooling 2h of room temperature, according to the GB/T2790-1995 test, the peel strength test after initial bonding strength and thermal ageing are processed the results are shown in Table 2.As can be seen from Table 2, the average load/width of sample is 3.245N/mm, and after thermal ageing is processed, average load/width is 3.016N/mm.
Embodiment 6:100 gram butyl reclaimed rubber (B) joins in the Haake rheometer, then adds 180 gram rosin and 800 gram barium sulfate, after mixing, adopts vulcanizing press to prepare 2mm slab-like material sample.Adopt dynamic mechanical analyzer (DMA) to carry out dynamic mechanical test to it.Test condition: frequency 11Hz, temperature--60~120 ℃, 3 ℃/min of temperature rise rate adopts stretching clamp, and test result is seen Fig. 6.As seen from Figure 6, the damping factor peak value of this material is 3.39, and peak value is positioned at 25.9 ℃.Dissipation factor is 8.8-53.8 ℃ greater than 1 temperature range, at the temperature range internal loss factor of 0.8 ℃ to 100 ℃ all greater than 0.5.
Adopt rotational viscosimeter to carry out the viscosity test to it, during mensuration, the instrument level is arranged on fixed support, then look the viscosity size, select suitable rotor and rotating speed, make reading at the 15%-85% of scale card, probe temperature is 180 ℃, and test result sees Table 3.As can be seen from Table 3, this material is 13500mPas at the rotation viscosity of 180 ℃.Adopt softening point apparatus to carry out the softening temperature test to material, test result sees Table 1, and as shown in Table 1, the softening temperature of this material is 78.1 ℃.
Adopt omnipotent test drawing machine to carry out mechanical test to it.Initial bonding strength is tested according to GB/T2790-1995.Sample is placed in 80 ℃ of constant temperature 336h, the cooling 2h of room temperature, according to the GB/T2790-1995 test, the peel strength test after initial bonding strength and thermal ageing are processed the results are shown in Table 2.As can be seen from Table 2, the average load/width of sample is 3.918N/mm, and after thermal ageing is processed, average load/width is 3.765N/mm.
Comparative Examples 1:100 gram isoprene-isobutylene rubber joins in the Haake torque rheometer, then adds 180 gram petroleum resin and 300 gram barium sulfate, after mixing, adopts vulcanizing press to prepare 2mm slab-like material sample.Adopt dynamic mechanical analyzer (DMA) to carry out dynamic mechanical test to it.Test condition: frequency 11Hz, temperature--60~120 ℃, 3 ℃/min of temperature rise rate adopts stretching clamp, and test result is seen Fig. 7.As seen from Figure 7, the damping factor peak value of this material is 2.79, and peak value is positioned at 19.8 ℃.
Comparative Examples 2:100 gram isoprene-isobutylene rubber joins in the Haake rheometer, then adds 180 gram rosin and 800 gram barium sulfate, after mixing, adopts vulcanizing press to prepare 2mm slab-like material sample.Adopt dynamic mechanical analyzer (DMA) to carry out dynamic mechanical test to it.Test condition: frequency 11Hz, temperature--60~120 ℃, 3 ℃/min of temperature rise rate adopts stretching clamp, and test result is seen Fig. 8.As seen from Figure 8, the damping factor peak value of this material is 3.20, and peak value is positioned at 26.9 ℃.Dissipation factor is 9.8-49.8 ℃ greater than 1 temperature range, at the temperature range internal loss factors of 2.8 ℃ to 66.8 ℃ all greater than 0.5.
Adopt rotational viscosimeter to carry out the viscosity test to it, during mensuration, the instrument level is arranged on fixed support, then look the viscosity size, select suitable rotor and rotating speed, make reading at the 15%-85% of scale card, probe temperature is 180 ℃, and test result sees Table 1.As can be seen from Table 1, this material is 117300mPas at the rotation viscosity of 180 ℃.Adopt softening point apparatus to carry out the softening temperature test to material, test result sees Table 1, and as shown in Table 1, the softening temperature of this material is 91.5 ℃.
Adopt omnipotent test drawing machine to carry out mechanical test to it.Initial bonding strength is tested according to GB/T2790-1995.Sample is placed in 80 ℃ of constant temperature 336h, the cooling 2h of room temperature, according to the GB/T2790-1995 test, the peel strength test after initial bonding strength and thermal ageing are processed the results are shown in Table 2.As can be seen from Table 2, the average load/width of sample is 2.711N/mm, and after thermal ageing is processed, average load/width is 2.853N/mm.
Table 1
? Rotary viscosity Softening temperature
Embodiment 5 8749mPa·s 81.5℃
Embodiment 6 13500mPa·s 78.1℃
Comparative Examples 2 117300mPa·s 91.5℃
Table 2
? Initial bonding strength Stripping strength after thermal ageing
Embodiment 5 3.245N/mm 3.016N/mm
Embodiment 6 3.918N/mm 3.765N/mm
Comparative Examples 2 2.711N/mm 2.853N/mm
In sum, butyl reclaimed rubber is that the damping sizing agent has good damping capacity, and the damping peak value can reach more than 4, and more than room temperature quite wide temperature range scope internal damping value greater than 0.3, apparently higher than the isoprene-isobutylene rubber damping material.In addition, the prepared damping material of the present invention has also had the bonding characteristic of sizing agent concurrently, and stripping strength can reach 3.245N/mm, is a kind of high performance damping sizing agent.

Claims (1)

1. a butyl reclaimed rubber is the damping sizing agent, it is characterized in that, said damping sizing agent prepares by the following method:
1) feed composition and ratio of quality and the number of copies are:
Butyl reclaimed rubber: 50-100 part
Isoprene-isobutylene rubber: 0-100 part
Damping imparting agent: 50-250 part
Mineral filler: 100-800 part,
The mooney viscosity ML[(1+4 of described butyl reclaimed rubber) 100 ℃] be 5-60,
Described damping imparting agent is petroleum resin or rosin,
Described mineral filler is barium sulfate or calcium carbonate;
2) add the Haake torque rheometer mixing described raw material in described ratio, temperature is 20-120 ℃, and the time is 10-30min, after mixing, and compressing tablet on vulcanizing press, making described butyl reclaimed rubber is the damping sizing agent.
CN2013100702866A 2013-03-06 2013-03-06 Reclaimed butyl rubber damping adhesive Pending CN103146322A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105038097A (en) * 2015-09-09 2015-11-11 青岛鑫铁成汽车配件有限公司 Self-adhesive butyl rubber and nitrile rubber blended damping material and preparing method thereof
CN105061912A (en) * 2015-09-09 2015-11-18 青岛鑫铁成汽车配件有限公司 Self-adhesive high-damping sound-absorbing butyl-rubber foamed material and preparation method thereof
CN109517537A (en) * 2018-10-17 2019-03-26 沈阳化工大学 A kind of butyl pressure sensitive adhesive containing C5 Petropols and butyl capsule reclaimed rubber

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CN102606414A (en) * 2011-01-24 2012-07-25 中山市邦达实业有限公司 Wind turbine blade with damping vibration attenuation structural layer and method for manufacturing wind turbine blade
JP2012243853A (en) * 2011-05-17 2012-12-10 Yokohama Rubber Co Ltd:The Reaction type hot melt sealing agent composition for solar cell
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105038097A (en) * 2015-09-09 2015-11-11 青岛鑫铁成汽车配件有限公司 Self-adhesive butyl rubber and nitrile rubber blended damping material and preparing method thereof
CN105061912A (en) * 2015-09-09 2015-11-18 青岛鑫铁成汽车配件有限公司 Self-adhesive high-damping sound-absorbing butyl-rubber foamed material and preparation method thereof
CN109517537A (en) * 2018-10-17 2019-03-26 沈阳化工大学 A kind of butyl pressure sensitive adhesive containing C5 Petropols and butyl capsule reclaimed rubber

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Application publication date: 20130612