CN109824989A - A kind of method that filling-modified basalt fibre prepares automobile primary driving seal rubber part - Google Patents
A kind of method that filling-modified basalt fibre prepares automobile primary driving seal rubber part Download PDFInfo
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- CN109824989A CN109824989A CN201910182668.5A CN201910182668A CN109824989A CN 109824989 A CN109824989 A CN 109824989A CN 201910182668 A CN201910182668 A CN 201910182668A CN 109824989 A CN109824989 A CN 109824989A
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Abstract
The invention discloses a kind of methods that filling-modified basalt fibre prepares automobile primary driving seal rubber part, titanate coupling agent is diluted with ethyl acetate, the pretreated basalt fibre of acetic acid is added thereto, after high-speed stirred, filter, dry titanate esters coupling modifier basalt fibre；It is added ethyl alcohol into ionic liquid, after magnetic agitation, is slowly added in carbon black-alcohol mixeding liquid while stirring, heating ultrasonic treatment, then forced air drying obtain ion liquid modified carbon black；Ethylene propylene diene rubber is put into opening rubber mixing machine and is rolled, basalt fibre, the ion liquid modified carbon black of naphthenic oil, zinc oxide, sulphur, stearic acid, antiaging agent, promotor, organic modification nano silica, polyacrylic acid lead powder and titanate esters coupling modifier is added, it continuess to mix, cutting is carried out to turn refining, through thin 5 times logical, mixing is uniformly dispersed, and obtains rubber compound；By it on rubber plate vulcanization machine sulfidization molding, obtain automobile primary driving seal rubber part.
Description
Technical field
The invention belongs to automobile rubber part fields, and in particular to a kind of filling-modified basalt fibre prepares automobile primary driving
The method of seal rubber part.
Background technique
Basalt fibre not only has good mechanical property as a kind of novel green material, and high temperature resistant is excellent
Different stability, good chemical resistance is easy to process, nontoxic, environmentally friendly and cheap, and has good low rolling resistance
Power.Basalt fibre, which is used for natural rubber, can be effectively reduced the fissipation factor of composite material, but due to basalt fibre
It is the characteristics of surface hydrophilic oleophobic, weak with the binding force of matrix, it is easy to reunite in rubber.In order to be mentioned while reducing fissipation factor
The mechanical property of high composite material needs to be modified basalt fibre.
Nano silica has many advantages, such as good chemical inertness, compatibility, stability, is widely used.But
It is that nano silica also has its disadvantage, especially its difficulties in dispersion, and matrix poor compatibility, to influence to fill out
Effect is filled, is limited its application, it is therefore desirable to which it is modified.Nano-silica surface has a large amount of reactive silicon groups,
Be conducive to carry out graft modification.
Summary of the invention
The purpose of the present invention is being directed to existing problem, provides a kind of filling-modified basalt fibre and prepare automobile primary drive
The method of dynamic sealing rubber part, the seal rubber part according to this method preparation have excellent mechanical property and shielding properties.
The present invention is achieved by the following technical solutions:
A kind of method that filling-modified basalt fibre prepares automobile primary driving seal rubber part, which is characterized in that including as follows
Step, following raw materials by weight:
(1) the titanate esters method of modifying of basalt fibre:
0.18-0.45 parts of titanate coupling agents are diluted with solvent ethyl acetate, then the pretreated basalt of 6-9 parts of acetic acid is fine
Dimension is added thereto, and after high-speed stirred 2-3h, is filtered, drying, is obtained the basalt fibre of titanate esters coupling modifier；
(2) preparation of ion liquid modified carbon black:
Ethyl alcohol is added into 63-77 parts of carbon blacks, is placed in 60-65 DEG C of water-bath and heats 30-40min, obtains carbon black-ethyl alcohol mixing
Liquid；It is added ethyl alcohol into 6.3-7.7 parts of ionic liquid BMI, after magnetic agitation 30-40min, is slowly added to carbon black-while stirring
In alcohol mixeding liquid, heating ultrasonic treatment 2-3h obtains ionic liquid structural reform then at forced air drying at 60-65 DEG C at 60-65 DEG C
Property carbon black；
Using the wet-process modified carbon black of ionic liquid BMI, the dispersibility of carbon black is improved, ionic liquid makes the friendship of vulcanized test specimens
Connection density, which has, largely to be improved, and tensile strength, tearing strength are promoted, and has certain improvement to wearability；
(3) preparation of automobile primary driving seal rubber part:
It will be rolled in 90-110 parts of ethylene propylene diene rubber investment opening rubber mixing machines, 13.5-16.5 parts of naphthenic oils of addition,
4.5-5.5 parts of zinc oxide, 1.35-1.65 parts of sulphur, 0.9-1.1 parts of stearic acid, 0.45-0.55 parts of antiaging agents, 0.45-0.55
Gains in part accelerant CZ, 3-4 parts of organic modification nano silicas, 20-25 parts of polyacrylic acid lead powders and (1), (2)
Material, continuess to mix, and carries out cutting and turns refining, and through thin 5 times logical, mixing is uniformly dispersed, and obtains rubber compound；By it in rubber plate vulcanization
Sulfidization molding on machine obtains automobile primary driving seal rubber part；
Using toluene as solvent, surface grafting organic modification, particle coupling agent obtained are carried out to nano silica with HK570
Grafting amount is high, and the dispersibility in rubber preferably, is significantly improved to the modified effect of rubber.
Further, in step (1) basalt fibre acetic acid preprocess method: 6-9 parts of basalt fibres are put in third
In ketone solution, low speed magnetic agitation 1-2h removal of impurities filters, is put into 60-65 DEG C of baking oven and dries 40-48h, places into the ice of 1mol/L
In acetic acid, mechanical stirring disperses 1-2h, takes out, and filters, cleans, dries 40-48h in 60-65 DEG C of baking oven, obtain acetic acid and locate in advance
The basalt fibre of reason.
Further, nano-silica surface graft-modification method in step (3): by 130-140 parts of toluene, 0.6-
Component A is mixed to obtain in 0.7 part of triethylamine, 0.6-0.7 parts of KH570, by 3-4 parts of silica and 130-170 parts of toluene ultrasounds
It after dispersing 30-40min, is added in component A, after reaction 10-12h is stirred at reflux at 60-65 DEG C, is centrifuged 5-10min, outwells
Supernatant is added in deionized water, ultrasonic disperse is freeze-dried to obtain organic modification nanometer after dehydrated alcohol eccentric cleaning
Silica.
Further, in step (3) polyacrylic acid lead powder preparation: be slowly added to 10-20 into 20-25 parts of lead oxide
The mixed solution of part acrylic acid and ethyl alcohol 1:1 filters off insoluble matter, slowly in 60-65 DEG C of water-bath after magnetic agitation reaction 1-2h
0.2-0.3 part initiator azodiisobutyronitriles are added, filter, dry polyacrylic acid lead powder.
Further, curing temperature is 160-190 DEG C, sulfide stress 5-10MPa, vulcanization time 30- in step (3)
35min。
The present invention has the advantage that compared with prior art
Acetic acid pretreatment modification basalt fibre is first used, acetic acid pre-processes the whole mechanical property to basalt fiber composite material
It can all increase, acetic acid pre-processes the dispersibility that basalt fibre can be improved, and on the one hand reduces carbon black filler network structure
It is formed, reduces and destroy energy consumed by its network structure, on the other hand increase the surface roughness of fiber, improve fiber
And the interaction of matrix hinders the interior friction between matrix macromolecular；Reuse the pretreatment of titanate coupling agent modified acetic acid
Basalt fibre, can be effectively reduced compound
The rolling resistance of material improves thermal stability.
Specific embodiment
Embodiment 1
A kind of method that filling-modified basalt fibre prepares automobile primary driving seal rubber part, which is characterized in that including as follows
Step, following raw materials by weight:
(1) the titanate esters method of modifying of basalt fibre:
0.18 part of titanate coupling agent is diluted with solvent ethyl acetate, then the pretreated basalt fibre of 6 parts of acetic acid is added
Wherein, it after high-speed stirred 2h, filters, drying, obtains the basalt fibre of titanate esters coupling modifier；
Wherein, the acetic acid preprocess method of basalt fibre: 6 parts of basalt fibres are put in acetone soln, low speed magnetic force stirs
1h removal of impurities to be mixed, filters, be put into 60 DEG C of baking ovens and dry 48h, place into the glacial acetic acid of 1mol/L, mechanical stirring disperses 1h, it takes out,
It filters, clean, dry 48h in 60 DEG C of baking ovens, obtain the pretreated basalt fibre of acetic acid；
(2) preparation of ion liquid modified carbon black:
Ethyl alcohol is added into 63 parts of carbon blacks, is placed in 60 DEG C of water-baths and heats 40min, obtain carbon black-alcohol mixeding liquid；To 6.3 parts
It is added ethyl alcohol in ionic liquid BMI, after magnetic agitation 30min, is slowly added in carbon black-alcohol mixeding liquid while stirring, 60
Heating ultrasonic treatment 3h, the forced air drying at 60 DEG C obtain ion liquid modified carbon black at DEG C；
(3) preparation of automobile primary driving seal rubber part:
It will be rolled in 90 parts of ethylene propylene diene rubber investment opening rubber mixing machines, 13.5 parts of naphthenic oils, 4.5 parts of oxidations be added
Zinc, 1.35 parts of sulphur, 0.9 part of stearic acid, 0.45 part of antiaging agent, 0.45 part of accelerant CZ, 3 parts of organic modification nano-silicas
Resulting material in SiClx, 20 parts of polyacrylic acid lead powders and (1), (2), continuess to mix, and carries out cutting and turns refining, mixed through thin 5 times logical
Conjunction is uniformly dispersed, and obtains rubber compound；By it on rubber plate vulcanization machine sulfidization molding, obtain automobile primary driving seal rubber
Part；
Wherein, nano-silica surface graft-modification method: 130 parts of toluene, 0.6 part of triethylamine, 0.6 part of KH570 are mixed
Component A is stirred to obtain, after 3 parts of silica and 130 parts of toluene ultrasonic disperse 30min, is added in component A, is stirred at 60 DEG C
After mixing back flow reaction 12h, it is centrifuged 5min, outwells supernatant, after dehydrated alcohol eccentric cleaning, is added in deionized water, ultrasound
Dispersion, is freeze-dried to obtain organic modification nano silica；
The preparation of polyacrylic acid lead powder: being slowly added to the mixed solution of 10 parts of acrylic acid and ethyl alcohol 1:1 into 20 parts of lead oxide,
In 60 DEG C of water-baths after magnetic agitation reaction 2h, insoluble matter is filtered off, 0.2 part of initiator azodiisobutyronitrile is slowly added to, filter,
Dry polyacrylic acid lead powder；
Curing temperature is 160 DEG C, sulfide stress 5MPa, vulcanization time 35min.
Embodiment 2
A kind of method that filling-modified basalt fibre prepares automobile primary driving seal rubber part, which is characterized in that including as follows
Step, following raw materials by weight:
(1) the titanate esters method of modifying of basalt fibre:
0.45 part of titanate coupling agent is diluted with solvent ethyl acetate, then the pretreated basalt fibre of 9 parts of acetic acid is added
Wherein, it after high-speed stirred 3h, filters, drying, obtains the basalt fibre of titanate esters coupling modifier；
Wherein, the acetic acid preprocess method of basalt fibre: 9 parts of basalt fibres are put in acetone soln, low speed magnetic force stirs
2h removal of impurities to be mixed, filters, be put into 65 DEG C of baking ovens and dry 40h, place into the glacial acetic acid of 1mol/L, mechanical stirring disperses 2h, it takes out,
It filters, clean, dry 40h in 65 DEG C of baking ovens, obtain the pretreated basalt fibre of acetic acid；
(2) preparation of ion liquid modified carbon black:
Ethyl alcohol is added into 77 parts of carbon blacks, is placed in 65 DEG C of water-baths and heats 30min, obtain carbon black-alcohol mixeding liquid；To 7.7 parts
It is added ethyl alcohol in ionic liquid BMI, after magnetic agitation 40min, is slowly added in carbon black-alcohol mixeding liquid while stirring, 65
Heating ultrasonic treatment 2h, the forced air drying at 65 DEG C obtain ion liquid modified carbon black at DEG C；
(3) preparation of automobile primary driving seal rubber part:
It will be rolled in 110 parts of ethylene propylene diene rubber investment opening rubber mixing machines, 16.5 parts of naphthenic oils, 5.5 parts of oxidations be added
Zinc, 1.65 parts of sulphur, 1.1 parts of stearic acid, 0.55 part of antiaging agent, 0.55 part of accelerant CZ, 4 parts of organic modification nano-silicas
Resulting material in SiClx, 25 parts of polyacrylic acid lead powders and (1), (2), continuess to mix, and carries out cutting and turns refining, mixed through thin 5 times logical
Conjunction is uniformly dispersed, and obtains rubber compound；By it on rubber plate vulcanization machine sulfidization molding, obtain automobile primary driving seal rubber
Part；
Wherein, nano-silica surface graft-modification method: 140 parts of toluene, 0.7 part of triethylamine, 0.7 part of KH570 are mixed
Component A is stirred to obtain, after 4 parts of silica and 170 parts of toluene ultrasonic disperse 40min, is added in component A, is stirred at 65 DEG C
After mixing back flow reaction 10h, it is centrifuged 10min, outwells supernatant, after dehydrated alcohol eccentric cleaning, is added in deionized water, ultrasound
Dispersion, is freeze-dried to obtain organic modification nano silica；
The preparation of polyacrylic acid lead powder: being slowly added to the mixed solution of 20 parts of acrylic acid and ethyl alcohol 1:1 into 25 parts of lead oxide,
In 65 DEG C of water-baths after magnetic agitation reaction 1h, insoluble matter is filtered off, 0.3 part of initiator azodiisobutyronitrile is slowly added to, filter,
Dry polyacrylic acid lead powder；
Curing temperature is 190 DEG C, sulfide stress 10MPa, vulcanization time 30min.
Comparative example 1
This comparative example 1 compared with Example 1, does not carry out pretreatment to basalt fibre using acetic acid in step (1) and changes
Property, method and step in addition to this is all the same.
Comparative example 2
This comparative example 2 compared with Example 2, is not added with polyacrylic acid lead powder in step (3), method step in addition to this
It is rapid all the same.
Blank ethylene propylene diene rubber of the control group without any modification
In order to compare the performance of automobile primary driving seal rubber part prepared by the present invention, to above-described embodiment 1, embodiment 2, comparison
The corresponding automobile primary driving seal rubber part obtained of embodiment 1,2 method of comparative example and control group are corresponding without appointing
The blank ethylene propylene diene rubber of what modification carries out performance detection according to professional standard, and tests seal rubber part pair
The ray mass attenuation coefficient of 105.31KeV, specific correlation data are as shown in table 1 below:
Table 1
| Project | Tensile strength | Elongation at break | Tearing strength | Shore A hardness | Mass attentuation coefficient |
| Embodiment 1 | 25MPa | 622% | 59KN/m | 81 degree | 1.58cm2/g |
| Embodiment 2 | 27MPa | 625% | 61KN/m | 83 degree | 1.56cm2/g |
| Comparative example 1 | 22MPa | 514% | 42KN/m | 72 degree | 1.57cm2/g |
| Comparative example 2 | 26MPa | 627% | 60KN/m | 82 degree | / |
| Control group | 20MPa | 497% | 33KN/m | 67 degree | / |
There is excellent tensile strength according to the automobile primary driving seal rubber part of the method for the present invention preparation, elongation at break, tear
Resistance to spalling, Shore A hardness；Pretreatment modification is not carried out to basalt fibre using acetic acid in comparative example 1, leads to automobile
The tensile strength of main driving seal rubber part, elongation at break, tearing strength, Shore A hardness reduce, but still better than control
The mechanical property of the blank ethylene propylene diene rubber of group；It is not added with polyacrylic acid lead powder in comparative example 2, causes to seal rubber
Glue part does not have shielding properties.
Claims (5)
1. a kind of method that filling-modified basalt fibre prepares automobile primary driving seal rubber part, which is characterized in that including such as
Lower step, following raw materials by weight:
(1) the titanate esters method of modifying of basalt fibre:
0.18-0.45 parts of titanate coupling agents are diluted with solvent ethyl acetate, then the pretreated basalt of 6-9 parts of acetic acid is fine
Dimension is added thereto, and after high-speed stirred 2-3h, is filtered, drying, is obtained the basalt fibre of titanate esters coupling modifier；
(2) preparation of ion liquid modified carbon black:
Ethyl alcohol is added into 63-77 parts of carbon blacks, is placed in 60-65 DEG C of water-bath and heats 30-40min, obtains carbon black-ethyl alcohol mixing
Liquid；It is added ethyl alcohol into 6.3-7.7 parts of ionic liquid BMI, after magnetic agitation 30-40min, is slowly added to carbon black-while stirring
In alcohol mixeding liquid, heating ultrasonic treatment 2-3h obtains ionic liquid structural reform then at forced air drying at 60-65 DEG C at 60-65 DEG C
Property carbon black；
(3) preparation of automobile primary driving seal rubber part:
It will be rolled in 90-110 parts of ethylene propylene diene rubber investment opening rubber mixing machines, 13.5-16.5 parts of naphthenic oils of addition,
4.5-5.5 parts of zinc oxide, 1.35-1.65 parts of sulphur, 0.9-1.1 parts of stearic acid, 0.45-0.55 parts of antiaging agents, 0.45-0.55
Gains in part accelerant CZ, 3-4 parts of organic modification nano silicas, 20-25 parts of polyacrylic acid lead powders and (1), (2)
Material, continuess to mix, and carries out cutting and turns refining, and through thin 5 times logical, mixing is uniformly dispersed, and obtains rubber compound；By it in rubber plate vulcanization
Sulfidization molding on machine obtains automobile primary driving seal rubber part.
2. the side that a kind of filling-modified basalt fibre according to claim 1 prepares automobile primary driving seal rubber part
Method, which is characterized in that the acetic acid preprocess method of basalt fibre in step (1):
6-9 parts of basalt fibres are put in acetone soln, low speed magnetic agitation 1-2h removal of impurities filters, is put into 60-65 DEG C of baking oven
Middle baking 40-48h, places into the glacial acetic acid of 1mol/L, and mechanical stirring disperses 1-2h, takes out, and filters, cleans, dries in 60-65 DEG C
40-48h is dried in case, obtains the pretreated basalt fibre of acetic acid.
3. the side that a kind of filling-modified basalt fibre according to claim 1 prepares automobile primary driving seal rubber part
Method, which is characterized in that nano-silica surface graft-modification method in step (3):
Component A is mixed to obtain in 130-140 parts of toluene, 0.6-0.7 parts of triethylamines, 0.6-0.7 parts of KH570, by 3-4 parts of dioxies
After SiClx and 130-170 parts of toluene ultrasonic disperse 30-40min, it is added in component A, reaction is stirred at reflux at 60-65 DEG C
After 10-12h, it is centrifuged 5-10min, outwells supernatant, after dehydrated alcohol eccentric cleaning, is added in deionized water, ultrasonic disperse,
It is freeze-dried to obtain organic modification nano silica.
4. the side that a kind of filling-modified basalt fibre according to claim 1 prepares automobile primary driving seal rubber part
Method, which is characterized in that the preparation of polyacrylic acid lead powder in step (3):
The mixed solution of 10-20 parts of acrylic acid and ethyl alcohol 1:1 is slowly added into 20-25 parts of lead oxide, in 60-65 DEG C of water-bath
After magnetic agitation reacts 1-2h, insoluble matter is filtered off, is slowly added to 0.2-0.3 part initiator azodiisobutyronitriles, filtered, is dry
Polyacrylic acid lead powder.
5. the side that a kind of filling-modified basalt fibre according to claim 1 prepares automobile primary driving seal rubber part
Method, which is characterized in that curing temperature is 160-190 DEG C, sulfide stress 5-10MPa, vulcanization time 30- in step (3)
35min。
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| CN113429640A (en) * | 2021-07-02 | 2021-09-24 | 鞍钢集团矿业有限公司 | Rubber composite material containing modified basalt fibers and preparation method thereof |
| CN113861460A (en) * | 2021-10-27 | 2021-12-31 | 西华大学 | Basalt fiber/polypropylene composite material based on surface roughened interface enhancement and preparation method thereof |
| CN114753152A (en) * | 2019-12-29 | 2022-07-15 | 河北新尔特橡塑密封有限公司 | Titanate modified polypropylene fiber, preparation method and application thereof, heat-shrinkage-resistant sealing ring and preparation method thereof |
| CN114891270A (en) * | 2022-06-17 | 2022-08-12 | 山东海科创新研究院有限公司 | Modified basalt fiber, polysulfone composite material with good weather resistance and preparation method thereof |
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| CN114753152A (en) * | 2019-12-29 | 2022-07-15 | 河北新尔特橡塑密封有限公司 | Titanate modified polypropylene fiber, preparation method and application thereof, heat-shrinkage-resistant sealing ring and preparation method thereof |
| CN112281540A (en) * | 2020-09-11 | 2021-01-29 | 广东维敏特科技有限公司 | Emulsion type coating for thermal sensitive paper and preparation method thereof |
| CN113429640A (en) * | 2021-07-02 | 2021-09-24 | 鞍钢集团矿业有限公司 | Rubber composite material containing modified basalt fibers and preparation method thereof |
| CN113861460A (en) * | 2021-10-27 | 2021-12-31 | 西华大学 | Basalt fiber/polypropylene composite material based on surface roughened interface enhancement and preparation method thereof |
| CN113861460B (en) * | 2021-10-27 | 2023-05-05 | 西华大学 | Basalt fiber/polypropylene composite material based on surface roughened interface enhancement and preparation method thereof |
| CN114921029A (en) * | 2022-02-21 | 2022-08-19 | 镇江市华银仪表电器有限公司 | High-toughness oil-resistant waterproof cable material and preparation method thereof |
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| CN114891270A (en) * | 2022-06-17 | 2022-08-12 | 山东海科创新研究院有限公司 | Modified basalt fiber, polysulfone composite material with good weather resistance and preparation method thereof |
| CN114891270B (en) * | 2022-06-17 | 2023-08-25 | 山东海科创新研究院有限公司 | Modified basalt fiber polysulfone composite material with good weather resistance and preparation method thereof |
| CN115806777A (en) * | 2022-12-22 | 2023-03-17 | 西南石油大学 | Basalt fiber reinforced ethylene propylene diene monomer waterproof coiled material and preparation method thereof |
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Application publication date: 20190531 |