CN102504338B - Branch-shaped damping agent and preparation method and use thereof - Google Patents
Branch-shaped damping agent and preparation method and use thereof Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- 239000001257 hydrogen Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 15
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 14
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 12
- 229910000077 silane Inorganic materials 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 239000005864 Sulphur Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims description 7
- 150000002431 hydrogen Chemical class 0.000 claims description 7
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 7
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 7
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 7
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 7
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- VHOQXEIFYTTXJU-UHFFFAOYSA-N Isobutylene-isoprene copolymer Chemical group CC(C)=C.CC(=C)C=C VHOQXEIFYTTXJU-UHFFFAOYSA-N 0.000 claims description 4
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- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
The invention discloses a branch-shaped damping agent and a preparation method and use thereof. The damping agent is formed by condensing branch-shaped organic montmorillonoid and hindered phenol. The preparation method of the damping agent comprises the following steps: reacting the branch-shaped organic montmorillonoid and the hindered phenol for 2 to 3 hours at 100 to 120 DEG C in a protective atmosphere of N2; vacuumizing till the vacuum degree reaches 120 to130pa, and continuing to react for 2 to 4 hours; ending the reaction, adding acetone to dissolve the product of the reaction completely, dripping the solution into ether, and settling; and filtering and drying. The branch-shaped damping agent disclosed by the invention can be used to prepare a damping rubber material. Compared with the prior art, the branch-shaped damping agent solves the migration problem of small molecular damping agents in a rubber substrate; a damping material prepared by the branch-shaped damping agent disclosed by the invention has the advantages of good damping effect, excellent mechanical and wear-resistance properties, low preparation cost, easy implementation and the like.
Description
Technical field
The present invention relates to a kind of damping agent and its preparation method and application, specifically, relate to a kind of dendriform damping agent and its preparation method and application, belong to the damping material technical field.
Background technology
Fast development along with modern science and technology and modern industry, mechanical means is tending towards high speed and automatization, therefore just inevitably produce the series of problems such as vibration, noise, repeated stress failure, thereby working accuracy and the quality product of impact machinery, the fatigue damage of acceleration mechanical structure, shorten the work-ing life of machinery, contaminate environment, the harm people's is healthy.Therefore, novel, the Efficient Damping material of development and exploitation excellent combination property are problem demanding prompt solutions.
Damping material is a kind ofly can absorb vibration mechanical energy and it is converted into the functional materials of heat energy, can be divided into piezoelectric damping composite material and organic hybrid damping material that visco-elastic damping material (polymer damping material), composite damping material, the high temperature resistant damping material of ceramic-like and high damping alloy material and development in recent years are got up.Wherein polymer damping material is most study, a most widely used class damping material.
At present, both at home and abroad the research of damping capacity is mainly concentrated on copolymerization and blending and modifying, interpenetrating polymer networks, conduction piezo-electric damping.But copolymerization and blending and modifying are only better to the material damping effect of using under the low temperature environment, are unfavorable for the high temperature damping; Interpenetrating polymer networks is mainly used in the coating, and the structural damping material is because removal of solvents is difficult, and cost is high, is difficult to big area and uses; For conduction piezo-electric type damping material, although its damping mechanism does not rely on the glass transition of polymkeric substance, because not mating between inorganic fill particle and the polymeric matrix, effciency of energy transfer is lower, and shock attenuation result is not good, can't satisfy actual needs.
Therefore, be necessary to study various damping vibration attenuation mechanism and various factor to the impact of damping vibration attenuation effect, rationally utilize the strong point of various damping vibration attenuation mechanism, explore a kind of novel damping noise reducing damping material that can satisfy the required high damping requirement of Practical Project, this all has very important realistic meaning to the raising of production and quality product to the improvement of people's living environment and the cost of reduction maintenance, maintenance and equipment replacement.
Summary of the invention
For the existing the problems referred to above of prior art and demand, the purpose of this invention is to provide good dendriform damping agent of a kind of damping and its preparation method and application.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of dendriform damping agent is to be carried out condensation reaction and got by dendriform organo montmorillonite and hindered phenol.
A kind of preparation method of described dendriform damping agent comprises the steps: at N
2Protection is lower, makes dendriform organo montmorillonite and hindered phenol 100~120 ℃ of reactions 2~3 hours; Being evacuated to vacuum tightness is 120~130pa, continues reaction 2~4 hours again; Finish reaction, add acetone product is dissolved fully, then be added dropwise in the ether and precipitate; Filter, drying namely gets described dendriform damping agent.
The mass ratio of described dendriform organo montmorillonite and hindered phenol is preferably 1: 16~and 1: 4.
The volume ratio of described ether and acetone is preferably 1: 1~and 3: 1.
Described drying is recommended as 80~100 ℃ of vacuum-dryings 3~5 hours.
The preparation of described dendriform organo montmorillonite is recommended to comprise the steps:
A) preparation organo montmorillonite
It is in 40~60% the aqueous ethanolic solution that the mixture of organise intercalator and inorganic polynite is added volumetric concentration, 70~90 ℃ of lower reactions after 2~3 hours, carries out vacuum-drying and gets in 70~100 ℃;
B) preparation 11-hydrogen full methyl isophthalic acid-six silica alkanol
Octamethylcyclotetrasiloxane and methyl hydrogen dichlorosilane are added in the acetic acid, at room temperature and logical N
2Stir in the situation after 20~40 minutes and be warming up to 40~60 ℃, be incubated and dewater after 3~5 hours and get;
C) preparation 9-chloro-1, full methyl nine silane of 17-dihydro
With step b) the pure and mild trimethylchlorosilane of 11-hydrogen full methyl isophthalic acid-six siloxanes that makes adds in the pyridine, at logical N
2Stir in the situation after 40~60 minutes and be warming up to 60~80 ℃, be incubated 2~4 hours and get;
D) preparation dendriform organo montmorillonite
At N
2Protection is lower, with step c) the 9-chloro-1 that makes, full methyl nine silane of 17-dihydro and tosic acid are added dropwise in the organo montmorillonite that step a) makes, drip and finish, in 100~120 ℃ of stirring reactions 8~10 hours, then vacuumize to remove unreacted monomer, the product that obtains with the methyl alcohol repetitive scrubbing again is until can't detect unreacted material and polymkeric substance in the washings; Product after the washing in 40~50 ℃ of vacuum-dryings 5~7 hours, is namely obtained the dendriform organo montmorillonite.
Described intercalator preferable methyl trichlorosilane or the dimethyldichlorosilane(DMCS) of organising.
In step 1 milliliter of aqueous ethanolic solution a): the add-on of the intercalator that organises is preferably 0.5~0.6 milliliter, and the add-on of inorganic polynite is preferably 0.5~1.5 gram.
Step b) in 1 milliliter of acetic acid: the add-on of octamethylcyclotetrasiloxane is preferably 0.01~0.03 mole, and the add-on of methyl hydrogen dichlorosilane is preferably 0.01~0.04 mole.
Step c) in 1 milliliter of pyridine: the add-on of 11-hydrogen full methyl isophthalic acid-six silica alkanol is preferably 0.01~0.04 mole, and the add-on of trimethylchlorosilane is preferably 0.005~0.02 mole.
Steps d) in: 9-chloro-1, the mass ratio of full methyl nine silane of 17-dihydro and organo montmorillonite be preferably 3: 1~6: 1, and the mass ratio of tosic acid and organo montmorillonite is preferably 0.015: 1~and 0.06: 1.
A kind of damping rubber material of using described dendriform damping agent preparation is characterized in that, adds described dendriform damping agent 10~15 mass parts in the rubber matrix of 100 mass parts.
As preferred version, composition and the proportioning of described damping rubber material are as follows:
Described rubber matrix is preferably any one or a few the combination in isoprene-isobutylene rubber, chlorinated butyl rubber, paracril, terpolymer EP rubber, styrene-butadiene rubber(SBR), the natural rubber.
Described vulcanizing agent is preferably sulphur.
A kind of described damping rubber material preparation method is that each of proportional quantity form added in mill, carries out mixing and gets at 40~60 ℃.
Compared with prior art, dendriform damping agent of the present invention has solved the migration problem of small molecules damping agent in rubber matrix, it is good that the damping rubber material that utilizes dendriform damping agent of the present invention to make has a damping, mechanical property is relative with wear resisting property good, reaches the advantages such as preparation cost is low, easy to implement.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed, complete explanation.
Used inorganic polynite is the product of the SMP trade mark of Zhejiang Feng Hong clay company limited production among the embodiment, and hindered phenol is the product of 2246 trades mark of Milan, Nanjing chemical industry company limited production.
Adopt transmission electron microscope method to observe the size of dendriform damping agent.
Adopt the thermogravimetry of " nano composite polymer/laminated silicate material theory and practice " (QiZongNeng, Shang Wenyu writes, Chemical Industry Press, 2002), the thermal weight loss core temperature of test branch form drag Buddhist nun agent.
Adopt the damping capacity of the DMA-242 type dynamic mechanical analyzer testing rubber of the anti-company's production of speeding of Germany.
Adopt tensile property and the wear hardness of GB 528-83 and GB/T1689-1998 testing rubber.
Embodiment 1
A) the inorganic polynite of 25g and 25mL METHYL TRICHLORO SILANE are joined in the there-necked flask, and adding 50mL volumetric concentration is 40% aqueous ethanolic solution, be heated to 70 ℃, stirring reaction 3 hours, then carry out solid-liquid separation, the solid that separation is obtained washs, and in 70 ℃ of vacuum-dryings, namely gets organo montmorillonite again;
B) 0.10mol octamethylcyclotetrasiloxane, 0.20mol methyl hydrogen dichlorosilane and 10mL acetic acid are added in the four-hole boiling flask, at room temperature and logical N
2In the situation, be warming up to 40 ℃ of insulation 5h behind the stirring 20min, the 10min that then dewaters obtains a kind of colourless transparent liquid, namely gets 11-hydrogen full methyl isophthalic acid-six silica alkanol;
C) with in 0.20mol 11-hydrogen full methyl isophthalic acid-six silica alkanol and 0.10mol trimethylchlorosilane and the 10mL pyridine adding four-hole boiling flask, at room temperature and logical N
2In the situation, be warming up to 60 ℃ of insulation 4h behind the stirring 40min, obtain a kind of colourless transparent liquid, namely get 9-chloro-1, full methyl nine silane of 17-dihydro;
D) at N
2Protection is lower, with 40g 9-chloro-1, full methyl nine silane of 17-dihydro and 0.3g tosic acid are added dropwise in the 10g organo montmorillonite, drip and finish, in 100 ℃ of violent stirring 10h, then vacuumize to remove unreacted monomer, the solid product that obtains with the methyl alcohol repetitive scrubbing is until can't detect unreacted material and polymkeric substance in washings; Solid product after the washing in 40 ℃ of vacuum-drying 7h, is namely got the dendriform organo montmorillonite;
E) at N
2Protection is lower, 10g dendriform organo montmorillonite and 40g hindered phenol is mixed, in 100 ℃ of reaction 3h, then being evacuated to vacuum tightness is 130pa, continue reaction 2h, add 10mL acetone product is dissolved fully, and then dropwise splash in the 10mL ether and precipitate; Filter, 80 ℃ of vacuum-dryings 5 hours, namely get the dendriform damping agent;
F) 100g isoprene-isobutylene rubber, 2g sulphur, 1g captax, 0.3g Vulcanization accelerator TMTD, 0.5g stearic acid, 3g zinc oxide, 1g antioxidant A, 10g dendriform damping agent are added in the mill, carry out mixingly at 40 ℃, namely get damping rubber material of the present invention.
The test data of the median size of dendriform damping agent and thermal weight loss core temperature is shown in Table 1.
The test data of the dissipation factor of damping rubber material, tensile strength, elongation at break and abrasion volume is shown in Table 2.
Embodiment 2
A) the inorganic polynite of 60g and 33mL METHYL TRICHLORO SILANE are joined in the there-necked flask, and adding 60mL volumetric concentration is 50% aqueous ethanolic solution, be heated to 80 ℃, stirring reaction 2.5 hours, then carry out solid-liquid separation, the solid that separation is obtained washs, and in 80 ℃ of vacuum-dryings, namely gets organo montmorillonite again;
B) 0.20mol octamethylcyclotetrasiloxane, 0.30mol methyl hydrogen dichlorosilane and 15mL acetic acid are added in the four-hole boiling flask, at room temperature and logical N
2In the situation, be warming up to 50 ℃ of insulation 4h behind the stirring 30min, the 15min that then dewaters obtains a kind of colourless transparent liquid, namely gets 11-hydrogen full methyl isophthalic acid-six silica alkanol;
C) with in 0.30mol 11-hydrogen full methyl isophthalic acid-six silica alkanol and 0.15mol trimethylchlorosilane and the 15mL pyridine adding four-hole boiling flask, at room temperature and logical N
2In the situation, be warming up to 70 ℃ of insulation 3h behind the stirring 50min, obtain a kind of colourless transparent liquid, namely get 9-chloro-1, full methyl nine silane of 17-dihydro;
D) at N
2Protection is lower, with 50g 9-chloro-1, full methyl nine silane of 17-dihydro and 0.5g tosic acid are added dropwise in the 15g organo montmorillonite, drip and finish, in 110 ℃ of violent stirring 9h, then vacuumize to remove unreacted monomer, the solid product that obtains with the methyl alcohol repetitive scrubbing is until can't detect unreacted material and polymkeric substance in washings; Solid product after the washing in 45 ℃ of vacuum-drying 6h, is namely got the dendriform organo montmorillonite;
E) at N
2Protection is lower, 10g dendriform organo montmorillonite and 80g hindered phenol is mixed, in 110 ℃ of reaction 2.5h, then being evacuated to vacuum tightness is 125pa, continue reaction 3h, add 10mL acetone product is dissolved fully, and then dropwise splash in the 20mL ether and precipitate; Filter, 90 ℃ of vacuum-dryings 4 hours, namely get the dendriform damping agent;
F) 100g chlorinated butyl rubber, 2.5g sulphur, 1.2g captax, 0.4g Vulcanization accelerator TMTD, 0.8g stearic acid, 4g zinc oxide, 2g antioxidant A, 12g dendriform damping agent are added in the mill, carry out mixingly at 50 ℃, namely get damping rubber material of the present invention.
The test data of the median size of dendriform damping agent and thermal weight loss core temperature is shown in Table 1.
The test data of the dissipation factor of damping rubber material, tensile strength, elongation at break and abrasion volume is shown in Table 2.
Embodiment 3
A) the inorganic polynite of 105g and 42mL dimethyldichlorosilane(DMCS) are joined in the there-necked flask, and adding 70mL volumetric concentration is 60% aqueous ethanolic solution, be heated to 90 ℃, stirring reaction 2 hours, then carry out solid-liquid separation, the solid that separation is obtained washs, and in 90 ℃ of vacuum-dryings, namely gets organo montmorillonite again;
B) 0.30mol octamethylcyclotetrasiloxane, 0.40mol methyl hydrogen dichlorosilane and 20mL acetic acid are added in the four-hole boiling flask, at room temperature and logical N
2In the situation, be warming up to 60 ℃ of insulation 3h behind the stirring 40min, the 20min that then dewaters obtains a kind of colourless transparent liquid, namely gets 11-hydrogen full methyl isophthalic acid-six silica alkanol;
C) with in 0.40mol 11-hydrogen full methyl isophthalic acid-six silica alkanol and 0.20mol trimethylchlorosilane and the 20mL pyridine adding four-hole boiling flask, at room temperature and logical N
2In the situation, be warming up to 60 ℃ of insulation 2h behind the stirring 60min, obtain a kind of colourless transparent liquid, namely get 9-chloro-1, full methyl nine silane of 17-dihydro;
D) at N
2Protection is lower, with 60g 9-chloro-1, full methyl nine silane of 17-dihydro and 0.6g tosic acid are added dropwise in the 20g organo montmorillonite, drip and finish, in 120 ℃ of violent stirring 8h, then vacuumize to remove unreacted monomer, the solid product that obtains with the methyl alcohol repetitive scrubbing is until can't detect unreacted material and polymkeric substance in washings; Solid product after the washing in 50 ℃ of vacuum-drying 5h, is namely got the dendriform organo montmorillonite;
E) at N
2Protection is lower, 10g dendriform organo montmorillonite and 160g hindered phenol is mixed, in 120 ℃ of reaction 2h, then being evacuated to vacuum tightness is 120pa, continue reaction 4h, add 10mL acetone product is dissolved fully, and then dropwise splash in the 30mL ether and precipitate; Filter, 100 ℃ of vacuum-dryings 3 hours, namely get the dendriform damping agent;
F) 100g paracril, 3g sulphur, 1.5g captax, 0.5g Vulcanization accelerator TMTD, 1.0g stearic acid, 5g zinc oxide, 3g antioxidant A, 15g dendriform damping agent are added in the mill, carry out mixingly at 60 ℃, namely get damping rubber material of the present invention.
The test data of the median size of dendriform damping agent and thermal weight loss core temperature is shown in Table 1.
The test data of the dissipation factor of damping rubber material, tensile strength, elongation at break and abrasion volume is shown in Table 2.
Comparative Examples 1
100g isoprene-isobutylene rubber, 2g sulphur, 1g captax, 0.3g Vulcanization accelerator TMTD, 0.5g stearic acid, 3g zinc oxide, 1g antioxidant A and 10g hindered phenol are added in the mill, carry out mixingly at 40 ℃, namely get existing damping rubber material.
The test data of the dissipation factor of prepared damping rubber material, tensile strength, elongation at break and abrasion volume is shown in Table 2.
Comparative Examples 2
100g chlorinated butyl rubber, 2.5g sulphur, 1.2g captax, 0.4g Vulcanization accelerator TMTD, 0.8g stearic acid, 4g zinc oxide, 2g antioxidant A, 12g hindered phenol are added in the mill, carry out mixingly at 50 ℃, namely get existing damping rubber material.
The test data of the dissipation factor of prepared damping rubber material, tensile strength, elongation at break and abrasion volume is shown in Table 2.
Comparative Examples 3
100g paracril, 3g sulphur, 1.5g captax, 0.5g Vulcanization accelerator TMTD, 1.0g stearic acid, 5g zinc oxide, 3g antioxidant A, 15g hindered phenol are added in the mill, carry out mixingly at 60 ℃, namely get existing damping rubber material.
The test data of the dissipation factor of prepared damping rubber material, tensile strength, elongation at break and abrasion volume is shown in Table 2.
The median size of table 1 dendriform damping agent and thermal weight loss core temperature
Sample | Median size/nm | The thermal weight loss core temperature/℃ |
Embodiment 1 | 30~50 | 250~300 |
Embodiment 2 | 50~70 | 300~350 |
Embodiment 3 | 70~90 | 350~400 |
By as seen from Table 1: dendriform damping agent provided by the present invention is nano material, has higher thermal stability.
The performance test data of table 2 damping rubber material
By as seen from Table 2: the damping rubber material effectiveness in vibration suppression that the present invention obtains is excellent, and mechanical property and wear resisting property are good.
What be necessary at last to illustrate is: above embodiment only is used for that the invention will be further described; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (16)
1. dendriform damping agent is characterized in that: be to be carried out condensation reaction and got by dendriform organo montmorillonite and hindered phenol.
2. the preparation method of a dendriform damping agent claimed in claim 1 is characterized in that, comprises the steps: at N
2Protection is lower, makes dendriform organo montmorillonite and hindered phenol 100~120 ℃ of reactions 2~3 hours; Being evacuated to vacuum tightness is 120~130pa, continues reaction 2~4 hours again; Finish reaction, add acetone product is dissolved fully, then be added dropwise in the ether and precipitate; Filter, drying namely gets described dendriform damping agent.
3. the preparation method of dendriform damping agent according to claim 2, it is characterized in that: the mass ratio of described dendriform organo montmorillonite and hindered phenol is 1: 16~1: 4.
4. the preparation method of dendriform damping agent according to claim 2, it is characterized in that: the volume ratio of described ether and acetone is 1: 1~3: 1.
5. the preparation method of dendriform damping agent according to claim 2, it is characterized in that: described drying is 80~100 ℃ of vacuum-dryings 3~5 hours.
6. the preparation method of dendriform damping agent according to claim 2 is characterized in that, the preparation of described dendriform organo montmorillonite comprises the steps:
A) preparation organo montmorillonite
It is in 40~60% the aqueous ethanolic solution that the mixture of organise intercalator and inorganic polynite is added volumetric concentration, 70~90 ℃ of lower reactions after 2~3 hours, carries out vacuum-drying and gets in 70~100 ℃;
B) preparation 11-hydrogen full methyl isophthalic acid-six silica alkanol
Octamethylcyclotetrasiloxane and methyl hydrogen dichlorosilane are added in the acetic acid, at room temperature and logical N
2Stir in the situation after 20~40 minutes and be warming up to 40~60 ℃, be incubated and dewater after 3~5 hours and get;
C) preparation 9-chloro-1, full methyl nine silane of 17-dihydro
With step b) the pure and mild trimethylchlorosilane of 11-hydrogen full methyl isophthalic acid-six siloxanes that makes adds in the pyridine, at logical N
2Stir in the situation after 40~60 minutes and be warming up to 60~80 ℃, be incubated 2~4 hours and get;
D) preparation dendriform organo montmorillonite
At N
2Protection is lower, with step c) the 9-chloro-1 that makes, full methyl nine silane of 17-dihydro and tosic acid are added dropwise in the organo montmorillonite that step a) makes, drip and finish, in 100~120 ℃ of stirring reactions 8~10 hours, then vacuumize to remove unreacted monomer, the product that obtains with the methyl alcohol repetitive scrubbing again is until can't detect unreacted material and polymkeric substance in the washings; Product after the washing in 40~50 ℃ of vacuum-dryings 5~7 hours, is namely obtained the dendriform organo montmorillonite.
7. the preparation method of dendriform damping agent according to claim 6, it is characterized in that: the described intercalator that organises is METHYL TRICHLORO SILANE or dimethyldichlorosilane(DMCS).
8. the preparation method of dendriform damping agent according to claim 6 is characterized in that, in step 1 milliliter of aqueous ethanolic solution a): the add-on of the intercalator that organises is 0.5~0.6 milliliter, and the add-on of inorganic polynite is 0.5~1.5 gram.
9. the preparation method of dendriform damping agent according to claim 6 is characterized in that, step b) 1 milliliter of acetic acid in: the add-on of octamethylcyclotetrasiloxane is 0.01~0.03 mole, and the add-on of methyl hydrogen dichlorosilane is 0.01~0.04 mole.
10. the preparation method of dendriform damping agent according to claim 6, it is characterized in that, step c) in 1 milliliter of pyridine: the add-on of 11-hydrogen full methyl isophthalic acid-six silica alkanol is 0.01~0.04 mole, and the add-on of trimethylchlorosilane is 0.005~0.02 mole.
11. the preparation method of dendriform damping agent according to claim 6, it is characterized in that, steps d) in: 9-chloro-1, the mass ratio of full methyl nine silane of 17-dihydro and organo montmorillonite is 3: 1~6: 1, the mass ratio of tosic acid and organo montmorillonite is 0.015: 1~0.06: 1.
12. an application rights requires the damping rubber material of 1 described dendriform damping agent preparation, it is characterized in that: in the rubber matrix of 100 mass parts, add described dendriform damping agent 10~15 mass parts.
14. damping rubber material according to claim 13 is characterized in that: described rubber matrix is selected from any one or a few the combination in isoprene-isobutylene rubber, chlorinated butyl rubber, paracril, terpolymer EP rubber, styrene-butadiene rubber(SBR), the natural rubber.
15. damping rubber material according to claim 13 is characterized in that: described vulcanizing agent is sulphur.
16. a claim 12 or 13 described damping rubber material preparation methods is characterized in that: each of proportional quantity formed add in mill, carry out mixing at 40~60 ℃.
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CN103205238B (en) * | 2013-03-14 | 2014-07-23 | 芜湖双翼机电实业有限公司 | Damping agent and application thereof |
CN103351539A (en) * | 2013-07-23 | 2013-10-16 | 中国工程物理研究院化工材料研究所 | Ethylene-propylene-diene monomer rubber/montmorillonite nanocomposite and preparation method thereof |
CN104292506B (en) * | 2014-10-03 | 2017-06-06 | 上海工程技术大学 | A kind of hyperbranched damping agent and its preparation method and application |
CN105199249B (en) * | 2015-10-27 | 2017-07-04 | 上海工程技术大学 | A kind of preparation method of the chlorinated butyl damping rubber containing modified montmorillonoid damping agent |
CN106188547B (en) * | 2016-07-08 | 2019-02-01 | 山东大学 | A kind of organosilicon damping additive and preparation method thereof |
CN106700292A (en) * | 2016-12-16 | 2017-05-24 | 吴中区穹窿山天仲高分子材料技术研究所 | High-elasticity high molecular material |
CN110128704B (en) * | 2019-06-06 | 2021-02-05 | 上海工程技术大学 | Hindered phenol modified montmorillonite damping agent and preparation method and application thereof |
CN110423410A (en) * | 2019-09-11 | 2019-11-08 | 衡水华瑞工程橡胶有限责任公司 | A kind of shock mount rubber montmorillonite composite material and preparation method thereof |
CN112876753B (en) * | 2021-01-21 | 2021-11-16 | 中国石油大学(北京) | Covalent organic framework/styrene butadiene rubber composite material and preparation method thereof |
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