CN115536850A - Aramid pulp modification method, reinforced rubber composite material and preparation method - Google Patents
Aramid pulp modification method, reinforced rubber composite material and preparation method Download PDFInfo
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- CN115536850A CN115536850A CN202110657708.4A CN202110657708A CN115536850A CN 115536850 A CN115536850 A CN 115536850A CN 202110657708 A CN202110657708 A CN 202110657708A CN 115536850 A CN115536850 A CN 115536850A
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Abstract
The invention discloses a preparation method of aramid pulp modified rubber, which comprises the following steps: respectively adding aramid pulp, a coupling agent, a fatty acid or aliphatic amide dispersing agent and hydroxypropyl-beta-cyclodextrin into a solvent, wherein the aramid pulp accounts for 15-35wt% of the mass of the solution, the coupling agent accounts for 2-5wt% of the mass of the solution, the fatty acid or aliphatic amide dispersing agent accounts for 2-5wt% of the mass of the solution, and the chitosan hydroxypropyl-beta-cyclodextrin accounts for 1-2.5wt% of the mass of the solution, and stirring to uniformly disperse the aramid pulp, the coupling agent, the fatty acid or aliphatic amide dispersing agent and the hydroxypropyl-beta-cyclodextrin; and standing the mixed solution, and drying at the temperature of 80-120 ℃ for 12-36h to obtain the dried modified aramid pulp material. The aramid pulp modified by the method has obvious effect of improving the mechanical property of the hydrogenated nitrile-butadiene rubber.
Description
Technical Field
The invention relates to the technical field of rubber reinforcement, in particular to a preparation method of aramid pulp modified rubber.
Background
Nitrile Butadiene Rubber (NBR) has the characteristics of oil resistance, easiness in modification and the like, is widely applied to various friction materials such as sealing elements, piston rings, water-lubricated bearings and the like, but has the limitation of wider application due to lower abrasion resistance. The inorganic filler, the organic filler and the fiber reinforced modified rubber are a simple method for improving the mechanical property and the friction property of the modified rubber.
The aramid pulp is a differentiated product of aramid fibers, and not only retains most excellent properties of the aramid fibers, such as heat resistance, wear resistance, size stability and the like; the aramid fiber has physical properties different from aramid fiber long fibers, such as fluffy micro-fiber cluster on the surface and pinpoint-shaped fibrillation of axial tail ends of the fibers, so that the specific surface area of the aramid fiber long fibers is large, and the potential contact surface of the aramid fiber long fibers with a reinforced matrix is large.
In the prior art, the aramid pulp is not ideal in mechanical property improvement effect after being added into a hydrogenated nitrile butadiene rubber sizing material.
Disclosure of Invention
The invention aims to provide an aramid pulp modification method, an aramid pulp reinforced rubber composite material and a preparation method, and solves one or more of the problems in the prior art.
On one hand, the invention provides a preparation method of aramid pulp modified rubber, which comprises the following steps:
respectively adding aramid pulp, a coupling agent, a fatty acid or aliphatic amide dispersing agent and hydroxypropyl-beta-cyclodextrin into a solvent, wherein the aramid pulp accounts for 15-35wt% of the mass of the solution, the coupling agent accounts for 2-5wt% of the mass of the solution, the fatty acid or aliphatic amide dispersing agent accounts for 2-5wt% of the mass of the solution, and the chitosan hydroxypropyl-beta-cyclodextrin accounts for 1-2.5wt% of the mass of the solution, and stirring to uniformly disperse the aramid pulp, the coupling agent, the fatty acid or aliphatic amide dispersing agent and the hydroxypropyl-beta-cyclodextrin;
and standing the mixed solution, and drying at the temperature of 80-120 ℃ for 12-36h to obtain the dried modified aramid pulp material.
In some embodiments, the coupling agent is one of KH-590, KH-580, KH-570, KH-560, or KH-550.
In some embodiments, the solvent is one or more of absolute ethanol, methanol, acetone, tetrahydrofuran, or an alkyl halide.
In some embodiments, the fatty acid-based or fatty amide-based dispersant is vinyl bis stearamide or glycerol monostearate.
In another aspect, the invention provides an aramid pulp reinforced rubber composite material, which comprises, by mass, 100 parts of hydrogenated nitrile rubber, 20 to 50 parts of carbon black, 1 to 5 parts of dicumyl peroxide and 0.5 to 2 parts of modified aramid.
In some embodiments, the modified aramid fiber comprises 100 parts by weight of hydrogenated nitrile rubber, 30 parts by weight of carbon black, 1.5 parts by weight of dicumyl peroxide and 1 part by weight of modified aramid fiber.
In another aspect, the present invention provides a method for preparing an aramid pulp reinforced rubber composite material, comprising:
banburying step: the initial temperature of the banburying is 60 ℃, and the rotor speed is 60r/min; adding hydrogenated nitrile rubber when banburying for 0 min; adding half of carbon black and half of modified aramid fiber when banburying for 1 min; banburying for 2.5min, and mixing the other half of carbon black and the modified aramid fiber; banburying for 4.0min, opening the upper ram and cleaning sequentially, and banburying for 6.5min, and discharging rubber;
open mixing: when the roller spacing of the open mill is 1.0mm, adding dicumyl peroxide, and tapping for 4 times; when the roller spacing of the open mill is 0.2mm, triangular bags are formed for 5 times; when the roller distance of the open mill is 1.6mm, the sheet is discharged and is parked.
The invention has the beneficial effects that:
the aramid pulp modified by the method has obvious effect of improving the mechanical property of the hydrogenated nitrile-butadiene rubber.
Drawings
Figure 1 is a graph of tensile stress performance data for formulations 1#, 2# and 3#.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are only for illustrating the performance of the present invention more clearly and are not limited to the following examples.
Example 1
A preparation method of aramid pulp modified rubber comprises the following steps:
respectively adding 225g of aramid pulp, 30g of coupling agent KH-550, 30g of stearic acid monoglyceride and 15g of hydroxypropyl-beta-cyclodextrin into 700g of solvent, wherein the aramid pulp accounts for 22.5wt% of the mass of the solution, the coupling agent KH-550 accounts for 3wt% of the mass of the solution, the stearic acid monoglyceride accounts for 3wt% of the mass of the solution, and the shell hydroxypropyl-beta-cyclodextrin accounts for 1.5wt% of the mass of the solution, and stirring to uniformly disperse the aramid pulp, the coupling agent KH-550, the stearic acid monoglyceride and the shell hydroxypropyl-beta-cyclodextrin;
and standing the mixed solution, and drying at 100 ℃ for 24 hours to obtain the dried modified aramid pulp material.
A preparation method of an aramid pulp reinforced rubber composite material comprises the following steps:
banburying step: the initial temperature of the banburying is 60 ℃, and the rotor speed is 60r/min; banburying for 0min, adding 1Kg of hydrogenated nitrile-butadiene rubber; adding 250g of carbon black and 10g of modified aramid fiber during banburying for 1 min; banburying for 2.5min, 250g of carbon black and 10g of modified aramid pulp; banburying for 4.0min, opening the upper top bolt and cleaning sequentially, and banburying for 6.5min, and discharging rubber;
open mixing: when the roller spacing of the open mill is 1.0mm, 50g of dicumyl peroxide is added, and the rubber tapping is carried out for 4 times; when the roller spacing of the open mill is 0.2mm, triangular bags are formed for 5 times; when the roller distance of the open mill is 1.6mm, the sheet is discharged and is parked.
Comparative example 1:
a preparation method of an aramid pulp reinforced rubber composite material comprises the following steps:
banburying step: the initial temperature of the banburying is 60 ℃, and the rotor speed is 60r/min; banburying for 0min, adding 1Kg of hydrogenated nitrile-butadiene rubber; adding 250g of carbon black and 10g of modified aramid fiber when banburying for 1 min; banburying for 2.5min, 250g of carbon black; banburying for 4.0min, opening the upper top bolt and cleaning sequentially, and banburying for 6.5min, and discharging rubber;
open mixing: when the roller spacing of the open mill is 1.0mm, 50g of dicumyl peroxide is added, and the rubber tapping is carried out for 4 times; when the roller spacing of the open mill is 0.2mm, triangular bags are formed for 5 times; when the roller distance of the open mill is 1.6mm, the sheet is discharged and is parked.
Comparative example 2:
a preparation method of an aramid pulp reinforced rubber composite material comprises the following steps:
banburying step: the initial temperature of the banburying is 60 ℃, and the rotor speed is 60r/min; banburying for 0min, adding 1Kg of hydrogenated nitrile-butadiene rubber; adding 250g of carbon black and 10g of modified aramid fiber during banburying for 1 min; banburying for 2.5min, 250g of carbon black and 10g of unmodified aramid pulp; banburying for 4.0min, opening the upper ram and cleaning sequentially, and banburying for 6.5min, and discharging rubber;
open mixing: when the roller spacing of the open mill is 1.0mm, 50g of dicumyl peroxide is added, and rubber tapping is performed for 4 times; when the roller spacing of the open mill is 0.2mm, packaging the mixture for 5 times by using a triangular bag; when the roller distance of the open mill is 1.6mm, the sheet is discharged and is parked.
Reference is made to comparative example 1 as formulation # 1, comparative example 2 as formulation # 2, and example 1 as formulation # 3. The rubbers No. 1, no. 2 and No. 3 were tested for tensile strength, stress at definite elongation and elongation at break using an electronic tensile machine, produced by Zwick, germany, according to the standard GB/T528-1998, the tear strength being determined in accordance with GB/T529-1999. Shore A hardness was measured according to GB/T531-1999.
The specific results are as follows:
| formulation of | 1# | 2# | 3# |
| Tensile strength/MPa | 19.6 | 20.9 | 22.5 |
| Elongation at break/%) | 583 | 590 | 613 |
| Stress at definite elongation (50%)/MPa | 1.4 | 2.2 | 3.7 |
| Stress at definite elongation (100%)/MPa | 2.0 | 3.3 | 4.8 |
| Stress at definite elongation (200%)/MPa | 6.1 | 7.0 | 8.8 |
| Stress at definite elongation (300%)/MPa | 11.7 | 11.0 | 13.1 |
| Tear Strength/N.mm-1 | 64 | 68 | 75 |
| Hardness of | 64 | 67 | 69 |
From the above table and fig. 1 it can be seen that:
compared with the aramid pulp which is not added in No. 1, the tensile strength, the elongation at break, the 50 percent stress at definite elongation, the 100 percent stress at definite elongation, the 200 percent stress at definite elongation, the tearing strength and the hardness of the hydrogenated nitrile rubber are improved to some extent in No. 2, but the improvement is not obvious, and the difference of the 300 percent stress at definite elongation is not large; probably because the surface of the aramid fiber pulp contains polar groups such as amino groups, sulfonic groups, amide groups, carboxylic groups and the like, the interaction between the aramid fiber pulp and the hydrogenated nitrile-butadiene rubber is poor, and the aramid fiber pulp is interacted, tangled and flocculated into a cluster shape, so that the aramid fiber pulp is poorly dispersed in the hydrogenated nitrile-butadiene rubber.
Compared with the method of adding the modified aramid pulp in the No. 3 material and the method of adding the unmodified aramid pulp in the No. 2 material, the tensile strength, the elongation at break, the 50% stress at definite elongation, the 100% stress at definite elongation, the 200% stress at definite elongation, the 300% stress at definite elongation, the tear strength and the hardness of the hydrogenated nitrile rubber are all obviously improved; probably because the modified aramid pulp is added with a hydroxypropyl-beta-cyclodextrin material which has the characteristics of external hydrophilicity and internal lipophilicity, stearic acid monoglyceride can be coated in the hydroxypropyl-beta-cyclodextrin, the external part is solidified on the surface of the aramid pulp through a covalent bond, the modified aramid fiber is added with hydrogenated nitrile butadiene rubber for refining, the coated stearic acid monoglyceride with a dispersing effect is gradually released in the refining process, the interaction between the aramid pulp and the hydrogenated nitrile butadiene rubber can be effectively improved, and the dispersibility of the aramid pulp in the hydrogenated nitrile butadiene rubber is improved.
In conclusion, the aramid pulp modified by the method has obvious effect of improving the mechanical property of the hydrogenated nitrile-butadiene rubber.
The above description is only a preferred form of the invention, and it should be noted that it is possible for a person skilled in the art to make several variations and modifications without departing from the inventive concept, and these should also be considered as within the scope of the invention.
Claims (7)
1. The aramid fiber pulp modification method is characterized by comprising the following steps of:
respectively adding aramid pulp, a coupling agent, a fatty acid or aliphatic amide dispersing agent and hydroxypropyl-beta-cyclodextrin into a solvent, wherein the aramid pulp accounts for 15-35wt% of the mass of the solution, the coupling agent accounts for 2-5wt% of the mass of the solution, the fatty acid or aliphatic amide dispersing agent accounts for 2-5wt% of the mass of the solution, and the chitosan hydroxypropyl-beta-cyclodextrin accounts for 1-2.5wt% of the mass of the solution, and stirring to uniformly disperse the aramid pulp, the coupling agent, the fatty acid or aliphatic amide dispersing agent and the hydroxypropyl-beta-cyclodextrin;
and standing the mixed solution, and drying at the temperature of 80-120 ℃ for 12-36h to obtain the dried modified aramid pulp material.
2. The method for preparing the aramid pulp-modified rubber according to claim 1, wherein the coupling agent is one of KH-590, KH-580, KH-570, KH-560 or KH-550.
3. The method for preparing the aramid pulp-modified rubber according to claim 1, wherein the solvent is one or more of absolute ethanol, methanol, acetone, tetrahydrofuran, and alkyl halide.
4. The method for preparing aramid pulp modified rubber as claimed in claim 2, wherein the fatty acid or fatty amide dispersing agent is vinyl bis stearamide or glyceryl monostearate.
5. The aramid pulp reinforced rubber composite material is characterized by comprising 100 parts of hydrogenated nitrile rubber, 20-50 parts of carbon black, 1-5 parts of dicumyl peroxide and 0.5-2 parts of modified aramid by mass parts.
6. The aramid pulp-reinforced rubber composite material of claim 5, comprising 100 parts by mass of hydrogenated nitrile rubber, 30 parts by mass of carbon black, 1.5 parts by mass of dicumyl peroxide and 1 part by mass of modified aramid.
7. The method for preparing the aramid pulp-reinforced rubber composite material according to claim 5 or 6, comprising:
banburying step: the initial temperature of the banburying is 60 ℃, and the rotating speed of a rotor is 60r/min; adding hydrogenated nitrile rubber when banburying for 0 min; adding half of carbon black and half of modified aramid fiber when banburying for 1 min; banburying for 2.5min, and mixing the other half of the carbon black and the modified aramid fiber; banburying for 4.0min, opening the upper ram and cleaning sequentially, and banburying for 6.5min, and discharging rubber;
open mixing: when the roller spacing of the open mill is 1.0mm, adding dicumyl peroxide, and tapping for 4 times; when the roller spacing of the open mill is 0.2mm, packaging the mixture for 5 times by using a triangular bag; when the roller distance of the open mill is 1.6mm, the sheet is discharged and is parked.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017048481A (en) * | 2015-09-03 | 2017-03-09 | 東レ株式会社 | Sizing agent coated reinforced fiber, manufacturing method of sizing agent coated reinforced fiber, prepreg and fiber reinforced composite material |
| CN107082918A (en) * | 2017-03-31 | 2017-08-22 | 太仓轮达汽车配件有限公司 | A kind of tyre rebuilding prevulcanized tire tread rubber and its preparation technology |
| CN109943087A (en) * | 2019-04-08 | 2019-06-28 | 张明军 | A kind of modified meerschaum fiber reinforced rubber pitch manufacturing method |
| CN110885461A (en) * | 2019-12-16 | 2020-03-17 | 山东非金属材料研究所 | Aramid pulp dispersion and preparation method thereof |
| CN112940305A (en) * | 2019-12-11 | 2021-06-11 | 北京化工大学 | Preparation method of aramid pulp masterbatch, masterbatch obtained by preparation method and application of masterbatch |
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- 2021-06-14 CN CN202110657708.4A patent/CN115536850A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017048481A (en) * | 2015-09-03 | 2017-03-09 | 東レ株式会社 | Sizing agent coated reinforced fiber, manufacturing method of sizing agent coated reinforced fiber, prepreg and fiber reinforced composite material |
| CN107082918A (en) * | 2017-03-31 | 2017-08-22 | 太仓轮达汽车配件有限公司 | A kind of tyre rebuilding prevulcanized tire tread rubber and its preparation technology |
| CN109943087A (en) * | 2019-04-08 | 2019-06-28 | 张明军 | A kind of modified meerschaum fiber reinforced rubber pitch manufacturing method |
| CN112940305A (en) * | 2019-12-11 | 2021-06-11 | 北京化工大学 | Preparation method of aramid pulp masterbatch, masterbatch obtained by preparation method and application of masterbatch |
| CN110885461A (en) * | 2019-12-16 | 2020-03-17 | 山东非金属材料研究所 | Aramid pulp dispersion and preparation method thereof |
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