CN109880188A - A kind of preparation method of automobile heat resistant rubber material - Google Patents
A kind of preparation method of automobile heat resistant rubber material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of automobile heat resistant rubber material, the swollen microcrystalline cellulose of alkali soluble is distributed in ethyl alcohol, stir evenly to obtain component A, ethyl orthosilicate, silane coupling agent are added in ethyl alcohol, component A is added dropwise, stirring in water bath reaction, ageing filter, dry microcrystalline cellulose-nano silicon dioxide hybridization body；The pretreated illite of pickling is added in silane coupling agent, it is cooling after reaction, it is centrifugated, washes, it is dry, grind to obtain silane coupler modified pickling illite；Natural rubber is added in mixer, add modified carbon black, zinc oxide, Rhein wax, anti-aging agent, modified multilayer graphene oxide and microcrystalline cellulose-nano silicon dioxide hybridization body, silane coupler modified pickling illite, mixing, then plus modified carbon black, stearic acid, mixing back glue；Sizing material is added in two-roll mill, after adding promotor, sulphur to mix, vulcanization beats triangle bag, bottom sheet obtains automobile rubber material.
Description
Technical field
The invention belongs to automobile rubber part fields, and in particular to a kind of preparation side of automobile heat resistant rubber material
Method.
Background technique
Microcrystalline cellulose is that a kind of source is wide, at low cost, renewable, degradable, low-density green filler, as one
The green filler of kind has been attracted wide attention in the application of rubber industry.But microcrystalline cellulose partial size is big, polarity is high, with non-pole
The compatibility of the rubber matrix of property is poor, therefore reinforcing effect is poor.The present invention uses absorption-reacting technique, in the micro- of swelling
Crystalline cellulose surface " insertion " and " cladding " nano silica, obtain microcrystalline cellulose-nano silicon dioxide hybridization body, to change
It is apt to its reinforcing effect to rubber.
The present invention has better affinity to organic matter by modifier modification illite, the modification illite of acquisition,
Modified illite is uniformly dispersed in rubber, and to illite, application has great significance in the composite for this.
Modern automobile industry proposes the heat-resistant air aging property under automobile-used rubber material high temperature resistant higher and higher
It is required that the long-term use temperature of car engine suspension be increased to from past 70-80 DEG C it is even higher close to 100 DEG C.
In terms of the damping angle of automobile engine, natural rubber is optimal rubber material, it is well known that the hot air of natural rubber
Ageing properties are very poor, therefore the high temperature resistance for improving natural rubber is just particularly important.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of preparation of automobile heat resistant rubber material is provided
Method, the rubber material according to this method preparation have excellent high temperature resistance, wear-resisting property and damping performance.
The present invention is achieved by the following technical solutions:
A kind of preparation method of automobile heat resistant rubber material, which is characterized in that include the following steps, following raw materials are pressed
Parts by weight meter:
(1) microcrystalline cellulose-nano silicon dioxide hybridization body preparation:
The 15-20 parts of swollen microcrystalline celluloses of alkali soluble are distributed in 90-110 parts of ethyl alcohol, stirring 10-20min is uniformly dispersed to obtain group
Divide A；15-20 parts of ethyl orthosilicates, 1-2 parts of silane coupling agent Si-69 are added in 55-65 parts of ethyl alcohol, component A is added dropwise,
Magnetic agitation reacts 50-60min in 60-65 DEG C of water-bath, is aged 30-40min, filters, in 80-85 DEG C of vacuum drying 5-6h, system
Obtain microcrystalline cellulose-nano silicon dioxide hybridization body；
First microcrystalline cellulose is swollen using sodium hydroxide as swelling agent, is then based on absorption-reacting technique principle, with
The moisture film of microcrystalline cellulose absorption is " microreactor ", and by sol-gel technique, nano-silica is generated in " microreactor "
SiClx obtains microcrystalline cellulose-nano silicon dioxide hybridization body, to improve its reinforcing effect to rubber；Hybrid is in rubber
It can be miniaturize in situ in process, and there is preferable interfacial interaction with rubber matrix, hence it is evident that improve tread rubber
The addition of composition machine performance and wear-resisting property, hybrid can also significantly improve the anti-slippery of tread rubber, while reduce rolling resistance
Power；
(2) the illitic method of silane coupler modified pickling:
The pretreated illite 1:100 of 5-10 parts of pickling is added in silane coupling agent KH560, in 80-85 DEG C of microwave reactor
Cooling after middle reaction 1-2h, centrifuge separation is added distilled water and is cleaned by ultrasonic, and 3-5 times repeatedly, the forced air drying 1- at 90-95 DEG C
2h grinds to obtain silane coupler modified pickling illite；
Using washing and two methods of pickling illite is pre-processed, make illite preferably with silane coupling agent KH560
Reaction, the modified illite of pickling have positive facilitation to reaction；
(3) preparation of automobile rubber material:
90-100 parts of natural rubbers are added in mixer, initial temperature is 65-75 DEG C, after mixing 1-2min, is added 30-33 parts
Modified carbon black, 3-3.5 part zinc oxide, 0.9-1 parts of Rhein waxes 654,1.8-2 parts of antioxidant 4020s, 1.8-2 parts of anti-aging agent RDs, 1-2
Resulting material in the modified multilayer graphene oxide of part and (1), (2), mixing 1-2min add 15-17 parts of modified carbon blacks, 1.8-
2 parts of stearic acid, mixing 3-5min back glue；Sizing material is added in two-roll mill, 1.35-1.5 parts of promotors are sequentially added
CBS, 0.45-0.5 parts of sulphur vulcanize at 160-170 DEG C after mixing, beat triangle bag 5 times, bottom sheet obtains the automobile
Use rubber material.
Further, in step (1) microcrystalline cellulose alkali swelling method: 15-20 parts of microcrystalline cellulose 1:2 are distributed to
In ethyl alcohol, the sodium hydroxide solution that 75-100 parts of mass fractions are 8% is added, is swollen 4-5h, filters, dry 10-12h, obtains alkali
The microcrystalline cellulose of swelling.
Further, 5-10 parts of illite powder illitic sulfuric acid refining preprocessing method in step (2): are pressed into solid-to-liquid ratio 1:
In the dilute hydrochloric acid solution that 40 investment molar concentrations are 1%, after 60-65 DEG C of stirred in water bath 1-2h, stands, cooling, be centrifuged 5-
10min outwells supernatant, and distilled water ultrasonic vibration is added and cleans 5-10min, then is centrifuged, cleans to neutrality, at 60-65 DEG C
Forced air drying 1-2h grinds to obtain the pretreated illite of pickling.
Further, in step (3) modified carbon black preparation: 3-7 parts of silane coupling agent Si69 1:5-10 are dissolved in quality
In the ethanol water that score is 70%, after mixing, 45-50 parts of carbon blacks is added and are sufficiently mixed, second of volatilizing in draught cupboard
Alcohol, heats 5-10min in 140-150 DEG C of insulating box, and cooling obtains modified carbon black.
Further, the preparation of multilayer graphene oxide is modified in step (3): into 1-2 parts of multilayer graphene oxides 1:
Dehydrated alcohol is added in 45-50, after ultrasonic disperse 1-2h, obtains component B, by silane coupling agent Si69 that volume ratio is 1:20:79,
Dehydrated alcohol, the deionized water magnetic agitation at 30-35 DEG C are 6 with careless acid for adjusting pH, continue to stir 5-6h hydrolysis, addition group
Divide B, 3-4h is reacted at 45-60 DEG C, centrifugation, alcohol are washed till neutrality, are dried in vacuo at 60-65 DEG C, obtain modified multilayer oxidation
Graphene.
The present invention has the advantage that compared with prior art
Using the modified multilayer graphene oxide of silane coupling agent Si69, silane coupling agent Si69 is successfully grafted on multilayer graphite oxide
On alkene, and multilayer graphene oxide surface wrinkles are more, are more dispersible in rubber matrix.The stretching for improving composite material is strong
Degree；Processing is modified to carbon black, to improve the compatibility of filler and rubber matrix and improve dispersion of the filler in rubber, glue
The physical and mechanical property of material is good.
Specific embodiment
Embodiment 1
A kind of preparation method of automobile heat resistant rubber material, which is characterized in that include the following steps, following raw materials are pressed
Parts by weight meter:
(1) microcrystalline cellulose-nano silicon dioxide hybridization body preparation:
15 parts of swollen microcrystalline celluloses of alkali soluble are distributed in 90 parts of ethyl alcohol, stirring 10min is uniformly dispersed to obtain component A；By 15 parts
Ethyl orthosilicate, 1 part of silane coupling agent Si-69 are added in 55 parts of ethyl alcohol, and component A, the magnetic agitation in 60 DEG C of water-baths is added dropwise
60min is reacted, 30min is aged, filters, in 80 DEG C of vacuum drying 6h, microcrystalline cellulose-nano silicon dioxide hybridization body is made；
Wherein, the alkali swelling method of microcrystalline cellulose: 15 parts of microcrystalline cellulose 1:2 are distributed in ethyl alcohol, and 75 parts of quality are added
The sodium hydroxide solution that score is 8% is swollen 4h, filters, dry 10h, obtains the swollen microcrystalline cellulose of alkali soluble；
(2) the illitic method of silane coupler modified pickling:
The pretreated illite 1:100 of 5 parts of pickling is added in silane coupling agent KH560, is reacted in 80 DEG C of microwave reactors
Cooling after 2h, centrifuge separation is added distilled water ultrasonic cleaning, 3 times repeatedly, the forced air drying 2h at 90 DEG C, grinds to obtain silane idol
Join the modified pickling illite of agent；
Wherein, illitic sulfuric acid refining preprocessing method: it is 1% that 5 parts of illite powder, which are put into molar concentration by solid-to-liquid ratio 1:40,
In dilute hydrochloric acid solution, after 60 DEG C of stirred in water bath 2h, stands, cooling, be centrifuged 5min, outwell supernatant, it is super that distilled water is added
Cleaning 5min is swung in acoustic shock, then is centrifuged, is cleaned to neutrality, and the forced air drying 2h at 60 DEG C grinds to obtain the pretreated illite of pickling；
(3) preparation of automobile rubber material:
90 parts of natural rubbers are added in mixer, initial temperature is 65 DEG C, and after mixing 2min, 30 parts of modified carbon blacks, 3 parts are added
Zinc oxide, 0.9 part of Rhein wax, 654,1.8 parts of antioxidant 4020s, 1.8 parts of anti-aging agent RDs, 1 part of modified multilayer graphene oxide and
(1), resulting material in (2), mixing 2min add 15 parts of modified carbon blacks, 1.8 parts of stearic acid, mixing 3min back glue；By glue
Material is added in two-roll mill, sequentially adds 1.35 parts of accelerator CBSs, 0.45 part of sulphur, after mixing, the sulphur at 160 DEG C
Change, beats triangle bag 5 times, bottom sheet obtains the automobile rubber material；
Wherein, 3 parts of silane coupling agent Si69 1:5 the preparation of modified carbon black: are dissolved in the ethanol water that mass fraction is 70%
In, after mixing, 45 parts of carbon blacks are added and are sufficiently mixed, volatilize ethyl alcohol in draught cupboard, heats in 140 DEG C of insulating boxs
10min, cooling obtain modified carbon black；
The preparation of modified multilayer graphene oxide: into 1 part of multilayer graphene oxide, dehydrated alcohol, ultrasonic disperse 1h is added in 1:45
Afterwards, component B is obtained, silane coupling agent Si69, dehydrated alcohol, the deionized water magnetic force at 30 DEG C for being 1:20:79 by volume ratio
Stirring is 6 with careless acid for adjusting pH, continues to stir 6h hydrolysis, component B is added, 4h is reacted at 45 DEG C, and centrifugation, alcohol are washed till neutrality,
It is dried in vacuo at 60 DEG C, obtains modified multilayer graphene oxide.
Embodiment 2
A kind of preparation method of automobile heat resistant rubber material, which is characterized in that include the following steps, following raw materials are pressed
Parts by weight meter:
(1) microcrystalline cellulose-nano silicon dioxide hybridization body preparation:
20 parts of swollen microcrystalline celluloses of alkali soluble are distributed in 110 parts of ethyl alcohol, stirring 20min is uniformly dispersed to obtain component A；By 20 parts
Ethyl orthosilicate, 2 parts of silane coupling agent Si-69 are added in 65 parts of ethyl alcohol, and component A, the magnetic agitation in 65 DEG C of water-baths is added dropwise
50min is reacted, 40min is aged, filters, in 85 DEG C of vacuum drying 5h, microcrystalline cellulose-nano silicon dioxide hybridization body is made；
Wherein, the alkali swelling method of microcrystalline cellulose: 20 parts of microcrystalline cellulose 1:2 are distributed in ethyl alcohol, and 100 parts of quality are added
The sodium hydroxide solution that score is 8% is swollen 5h, filters, dry 12h, obtains the swollen microcrystalline cellulose of alkali soluble；
(2) the illitic method of silane coupler modified pickling:
The pretreated illite 1:100 of 10 parts of pickling is added in silane coupling agent KH560, is reacted in 85 DEG C of microwave reactors
Cooling after 1h, centrifuge separation is added distilled water ultrasonic cleaning, 5 times repeatedly, the forced air drying 1h at 95 DEG C, grinds to obtain silane idol
Join the modified pickling illite of agent；
Wherein, illitic sulfuric acid refining preprocessing method: it is 1% that 10 parts of illite powder, which are put into molar concentration by solid-to-liquid ratio 1:40,
Dilute hydrochloric acid solution in, after 65 DEG C of stirred in water bath 1h, stand, cooling, be centrifuged 10min, outwell supernatant, distilled water is added
Ultrasonic vibration cleans 10min, then is centrifuged, cleans to neutrality, and the forced air drying 1h at 65 DEG C grinds to obtain the pretreated Erie of pickling
Stone；
(3) preparation of automobile rubber material:
100 parts of natural rubbers are added in mixers, initial temperature is 75 DEG C, after mixing 1min, be added 33 parts of modified carbon blacks,
3.5 parts of zinc oxide, 1 part of Rhein wax, 654,2 parts of antioxidant 4020s, 2 parts of anti-aging agent RDs, 2 parts of modified multilayer graphene oxides and
(1), resulting material in (2), mixing 1min add 17 parts of modified carbon blacks, 2 parts of stearic acid, mixing 3min back glue；By sizing material
It is added in two-roll mill, sequentially adds 1.5 parts of accelerator CBSs, 0.5 part of sulphur vulcanizes at 170 DEG C, beats after mixing
Triangle bag 5 times, bottom sheet obtains the automobile rubber material；
Wherein, 7 parts of silane coupling agent Si69 1:10 the preparation of modified carbon black: are dissolved in the ethanol water that mass fraction is 70%
In, after mixing, 50 parts of carbon blacks are added and are sufficiently mixed, volatilize ethyl alcohol in draught cupboard, heats in 150 DEG C of insulating boxs
5min, cooling obtain modified carbon black；
The preparation of modified multilayer graphene oxide: into 2 parts of multilayer graphene oxides, dehydrated alcohol, ultrasonic disperse 2h is added in 1:50
Afterwards, component B is obtained, silane coupling agent Si69, dehydrated alcohol, the deionized water magnetic force at 35 DEG C for being 1:20:79 by volume ratio
Stirring is 6 with careless acid for adjusting pH, continues to stir 5h hydrolysis, component B is added, 3h is reacted at 60 DEG C, and centrifugation, alcohol are washed till neutrality,
It is dried in vacuo at 65 DEG C, obtains modified multilayer graphene oxide.
Comparative example 1
This comparative example 1 compared with Example 1, does not carry out pickling pretreatment to illite in step (2), side in addition to this
Method step is all the same.
Comparative example 2
This comparative example 2 compared with Example 2, is not modified processing to carbon black in step (3), method step in addition to this
It is rapid all the same.
Blank natural rubber of the control group without any modification
In order to compare the performance of automobile rubber material prepared by the present invention, to above-described embodiment 1, embodiment 2, comparative example
1,2 method of comparative example corresponding obtained automobile rubber material and control group are corresponding without any modification
Blank natural rubber carries out performance detection according to professional standard, and sample is put into 100 DEG C of aging constant temperature oven and carries out heat
Air aging, specific correlation data are as shown in table 1 below:
Table 1
| Project | Tensile strength MPa | Heat resistant performance |
| Embodiment 1 | 28 | Aging 96h mechanical property is unchanged |
| Embodiment 2 | 29 | Aging 96h mechanical property is unchanged |
| Comparative example 1 | 28 | Aging 48h mechanical property reduces |
| Comparative example 2 | 13 | Aging 96h mechanical property is unchanged |
| Control group | 9 | Mechanical property reduces for 24 hours for aging |
There is excellent tensile strength and heat resistant performance according to the automobile rubber material of the method for the present invention preparation；Right
Than not carrying out pickling pretreatment to illite in embodiment 1, the tensile strength of rubber material is caused to weaken, but still better than control
The tensile strength of the blank natural rubber of group；Processing is not modified to carbon black in comparative example 2, leads to rubber material
Ageing-resistant performance reduces, but the heat resistant performance of the blank natural rubber still better than control group.
Claims (5)
1. a kind of preparation method of automobile heat resistant rubber material, which is characterized in that include the following steps, following raw materials
By weight:
(1) microcrystalline cellulose-nano silicon dioxide hybridization body preparation:
The 15-20 parts of swollen microcrystalline celluloses of alkali soluble are distributed in 90-110 parts of ethyl alcohol, stirring 10-20min is uniformly dispersed to obtain group
Divide A；15-20 parts of ethyl orthosilicates, 1-2 parts of silane coupling agent Si-69 are added in 55-65 parts of ethyl alcohol, component A is added dropwise,
Magnetic agitation reacts 50-60min in 60-65 DEG C of water-bath, is aged 30-40min, filters, in 80-85 DEG C of vacuum drying 5-6h, system
Obtain microcrystalline cellulose-nano silicon dioxide hybridization body；
(2) the illitic method of silane coupler modified pickling:
The pretreated illite 1:100 of 5-10 parts of pickling is added in silane coupling agent KH560, in 80-85 DEG C of microwave reactor
Cooling after middle reaction 1-2h, centrifuge separation is added distilled water and is cleaned by ultrasonic, and 3-5 times repeatedly, the forced air drying 1- at 90-95 DEG C
2h grinds to obtain silane coupler modified pickling illite；
(3) preparation of automobile rubber material:
90-100 parts of natural rubbers are added in mixer, initial temperature is 65-75 DEG C, after mixing 1-2min, is added 30-33 parts
Modified carbon black, 3-3.5 part zinc oxide, 0.9-1 parts of Rhein waxes 654,1.8-2 parts of antioxidant 4020s, 1.8-2 parts of anti-aging agent RDs, 1-2
Resulting material in the modified multilayer graphene oxide of part and (1), (2), mixing 1-2min add 15-17 parts of modified carbon blacks, 1.8-
2 parts of stearic acid, mixing 3-5min back glue；Sizing material is added in two-roll mill, 1.35-1.5 parts of promotors are sequentially added
CBS, 0.45-0.5 parts of sulphur vulcanize at 160-170 DEG C after mixing, beat triangle bag 5 times, bottom sheet obtains the automobile
Use rubber material.
2. a kind of preparation method of automobile heat resistant rubber material according to claim 1, which is characterized in that step
Suddenly in (1) microcrystalline cellulose alkali swelling method:
15-20 parts of microcrystalline cellulose 1:2 are distributed in ethyl alcohol, it is molten that the sodium hydroxide that 75-100 parts of mass fractions are 8% is added
Liquid is swollen 4-5h, filters, dry 10-12h, obtains the swollen microcrystalline cellulose of alkali soluble.
3. a kind of preparation method of automobile heat resistant rubber material according to claim 1, which is characterized in that step
Suddenly illitic sulfuric acid refining preprocessing method in (2):
5-10 parts of illite powder are put into the dilute hydrochloric acid solution that molar concentration is 1% by solid-to-liquid ratio 1:40, in 60-65 DEG C of water
It after stirring 1-2h in bath, stands, cooling, is centrifuged 5-10min, outwell supernatant, distilled water ultrasonic vibration is added and cleans 5-
10min, then be centrifuged, clean to neutrality, the forced air drying 1-2h at 60-65 DEG C grinds to obtain the pretreated illite of pickling.
4. a kind of preparation method of automobile heat resistant rubber material according to claim 1, which is characterized in that step
Suddenly in (3) modified carbon black preparation:
3-7 parts of silane coupling agent Si69 1:5-10 are dissolved in the ethanol water that mass fraction is 70%, after mixing, are added
Enter 45-50 parts of carbon blacks to be sufficiently mixed, volatilize ethyl alcohol in draught cupboard, and 5-10min is heated in 140-150 DEG C of insulating box, cooling
Obtain modified carbon black.
5. a kind of preparation method of automobile heat resistant rubber material according to claim 1, which is characterized in that step
Suddenly the preparation of multilayer graphene oxide is modified in (3):
Into 1-2 parts of multilayer graphene oxides, dehydrated alcohol is added in 1:45-50, after ultrasonic disperse 1-2h, component B is obtained, by body
Product magnetic agitation at 30-35 DEG C than the silane coupling agent Si69, dehydrated alcohol, deionized water for 1:20:79, is adjusted with oxalic acid
PH is 6, continues to stir 5-6h hydrolysis, component B is added, 3-4h is reacted at 45-60 DEG C, centrifugation, alcohol are washed till neutrality, in 60-65
It is dried in vacuo at DEG C, obtains modified multilayer graphene oxide.
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Cited By (1)
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Application publication date: 20190614 |