CN110885461B - Aramid pulp dispersion and preparation method thereof - Google Patents
Aramid pulp dispersion and preparation method thereof Download PDFInfo
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- CN110885461B CN110885461B CN201911305615.4A CN201911305615A CN110885461B CN 110885461 B CN110885461 B CN 110885461B CN 201911305615 A CN201911305615 A CN 201911305615A CN 110885461 B CN110885461 B CN 110885461B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/045—Reinforcing macromolecular compounds with loose or coherent fibrous material with vegetable or animal fibrous material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2307/00—Characterised by the use of natural rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
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Abstract
The invention relates to the technical field of pretreatment of reinforcing fibers for rubber and resin, in particular to an aramid pulp dispersion and a preparation method thereof.
Description
Technical Field
The invention relates to the technical field of pretreatment of reinforcing fibers for rubber and resin, in particular to an aramid pulp dispersion and a preparation method thereof.
Background
Aramid Pulp (hereinafter referred to as AP) is a highly fibrillated short fiber, not only has the characteristics of Aramid such as high modulus, high strength, high stability, toughness and the like, but also has a special three-dimensional structure and a higher specific surface area, and the microfiber of the Aramid Pulp can enable the Aramid Pulp to be anchored in a base material to generate a unique accordion effect, the reinforcing effect is superior to that of carbon black and white carbon black, the hysteresis heat generation is low, the Aramid Pulp can be used as a special filler to improve the strength and the wear resistance of the material, and the Aramid Pulp can be widely used in the fields of friction and sealing, such as brake pads, clutch pads and the like.
The excellent physical and chemical properties enable AP to have great application potential in the direction of prolonging the service life of a vibration damping product used in a harsh dynamic environment, but due to the surface chemical inertness and easy mutual entanglement of microfibers, the AP needs to be pretreated, and meanwhile, the problems of the interface action strength and dispersion of pulp and a matrix are solved, otherwise, the AP becomes a defect source of the vibration damping material and brings adverse effects.
At present, the pretreatment methods of AP are different according to the side emphasis, and can be divided into two types of methods, namely, emphasizing the dispersibility and emphasizing the interface strength:
1. pre-treatment method with attention paid to dispersibility
Patents US4514541 and EPA0272459 disclose a process for preparing AP pre-dispersed rubber, which comprises mixing AP and reinforcing filler such as carbon black at a certain ratio, stirring at high speed, adding into organic solution or liquid elastomer, stirring, and granulating.
In order to improve the dispersibility of AP in various matrixes, the patent CN1896369A discloses an AP pretreatment method, which comprises the steps of sequentially utilizing low-surface-energy inorganic isolation powder hollow glass beads and a lubricant phthalate compound to carry out powder isolation and lubrication infiltration on the AP so as to thoroughly isolate micro-fibers of the AP, and the AP has excellent dispersibility in various matrixes.
Patent CN102134394B discloses an AP dispersion and a preparation method thereof, the specific method is that AP is pre-dispersed in a dispersion solvent gasoline or ethyl acetate, stirred to be flocculent, then added with a separant white carbon black or pottery clay, silane or titanate coupling agent in sequence for dispersion and modification, then dissolved in a dispersion carrier coumarone resin or phenolic resin, desolventized and crushed to obtain the AP dispersion.
The method greatly improves the dispersion effect of AP in the matrix material, but the interface strength with the matrix is not obviously improved, and the method is only suitable for the fields of friction, static sealing and the like and is not suitable for vibration reduction and dynamic sealing.
2. Pretreatment method for emphasizing interface strength
The surface modification method of aramid fiber can be divided into physical modification and chemical modification. Wherein, the former is to treat the aramid fiber surface by physical technologies such as plasma, ultrasonic wave, ultraviolet ray and the like; the latter is to introduce active groups such as amido, hydroxyl, carboxyl and the like on the surface of the fiber through chemical reaction, and to improve the bonding strength between the aramid fiber and the matrix material through chemical bonding or polar action, and is mainly divided into methods such as surface chemical etching, surface grafting, coupling agent modification and the like. In addition, the interface action of the AP and the matrix can be enhanced through the viscosity treatment of the matrix material.
Patent EP0376623A2 discloses that polyisocyanate and epoxy resin are dissolved in a benzene organic solvent to prepare a mixed solution, and the mixed solution is used for carrying out surface modification treatment on aramid fibers at the temperature of 100-270 ℃.
Patent JP63-212364 mentions the addition of a certain amount of chlorophenol to a resorcinol-formaldehyde-latex dip to improve the adhesion of aramid to rubber.
The method effectively improves the interface strength of the aramid fiber and the matrix material, is suitable for surface treatment of aramid fiber long fibers and fabrics thereof, but is not beneficial to uniform dispersion of AP in the matrix.
As can be seen from the above, two methods for preprocessing an AP in the prior art have certain disadvantages, and a balanced effect cannot be obtained, so how to overcome the above difficulties becomes a problem to be solved by those skilled in the art.
Disclosure of Invention
The aramid pulp dispersion is reasonably mixed with a modifier, a coupling agent and a separant, chemical grafting modification is carried out on the inert surface of the aramid pulp through the modifier, the coupling agent and certain process steps, so that the aramid pulp can be bonded with matrix materials such as rubber, resin and the like, then the separant is selected for isolating and protecting the modified aramid pulp, and the obtained aramid pulp dispersion has good interface strength and dispersibility, and can be used as a reinforcing material to improve the crack expansion resistance of the matrix and improve the fatigue performance of a damping material.
The specific technical scheme of the invention is as follows:
the aramid pulp dispersion comprises the following main components in parts by weight:
10-20 parts of aramid pulp, 2-4 parts of modifier and 2-4 parts of coupling agent
0-20 parts of a release agent;
wherein the modifier is polyisocyanate;
the polyisocyanate is further an isocyanate substance containing two or more isocyanate groups, and can be one of toluene diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate and polymethylene polyphenyl polyisocyanate;
the coupling agent is silane coupling agent, such as one of KH-602, KH-590, KH-580, KH-570, KH-560 and KH-550;
the separant is calcium carbonate, talcum powder, carbon black or white carbon black.
In addition, the inventor also provides a preparation method of the aramid pulp dispersion, which comprises the following process steps:
1) uniformly mixing the modifier with the amount of the dispersing solvent which is 20-100 times of the modifier by mass;
2) stirring and dispersing aramid fiber pulp with a formula amount in the modifier dilute solution obtained in the step 1);
3) standing the mixed solution obtained in the step 2) for 10-30 h;
4) removing the solvent from the modified aramid pulp mixed solution obtained in the step 3) by adopting a negative pressure suction filtration or centrifugal drying mode, and then, placing the mixture in an environment with the temperature of 80-120 ℃ for heat treatment for 20-90 min;
5) uniformly mixing the coupling agent with the formula amount and a dispersion solvent with the mass being 20-100 times of that of the coupling agent;
6) stirring and dispersing the aramid pulp obtained in the step 4) in the coupling agent dilute solution obtained in the step 5);
7) standing the mixed solution obtained in the step 6) for 10-30 h;
8) carrying out desolventizing on the modified aramid pulp obtained in the step 7) by adopting a negative pressure suction filtration or centrifugal drying mode, and then, placing the modified aramid pulp in an environment with the temperature of 80-120 ℃ for heat treatment for 20-90 min;
9) adding the isolating agent with the formula amount into the modified aramid pulp obtained in the step 8), and uniformly mixing to obtain the aramid pulp dispersion.
The dispersing solvent adopted in the steps 1) and 5) is acetone or an alkane solvent;
the selected polyisocyanate modifier is an isocyanate substance containing two or more isocyanate groups, the two or more isocyanate groups on the molecule of the modifier have different activities due to steric hindrance and the like, and by combining the aramid pulp dispersion composition and the preparation method thereof provided by the invention, the isocyanate groups with higher activity on the polyisocyanate modifier can be grafted to the AP surface amide group preferentially by regulating the chemical reaction sequence of the components; under the action of steric hindrance, activity inhibition and the like, the isocyanate group with lower activity on the modifier does not react with the AP and is reserved, so that an active group such as amino or isocyanate group is introduced on the surface of the AP; the subsequent process steps of standing, heat treatment and the like can promote the coupling agent to be used as a bridge, and the modified AP and the matrix material generate chemical bonding or hydrogen bond action, so that the AP can be used as a reinforcing material to generate effective bonding with the matrix materials such as rubber, resin and the like; and the isolating agent is added in time after drying, so that the activated pulp dispersion can be isolated and protected, agglomeration is prevented, the dispersing agent has good dispersibility in the matrix material, and the storage is convenient.
The pulp dispersion is used for reinforcing and modifying materials such as rubber, resin and the like, can be uniformly dispersed in the matrix material and has good interface strength, the excellent physical and chemical properties of the aramid pulp are exerted, the crack expansion resistance of the matrix material is improved, the fatigue performance of the damping material is improved, and therefore the fatigue life of the material is effectively prolonged.
Detailed Description
The present invention is further illustrated below with reference to examples, which will enable those skilled in the art to more fully understand the present invention, but which are not intended to limit the invention in any way;
example 1
An aramid pulp dispersion and a preparation method thereof, the specific steps are as follows:
1) weighing 10 parts of aramid pulp, 2 parts of toluene diisocyanate serving as a modifier, KH-5602 parts of silane coupling agent and 10 parts of calcium carbonate serving as a separant; weighing 300 parts of acetone serving as a dispersion solvent;
2) uniformly mixing the modifier with acetone 60 times of the weight of the modifier;
3) stirring and dispersing aramid pulp in the modifier dilute solution obtained in the step 2);
4) standing the mixed solution obtained in the step 3) for 20 hours;
5) removing the solvent from the modified aramid pulp mixed solution obtained in the step 4) by adopting a negative pressure suction filtration mode, and then, placing the mixture in a temperature environment of 120 ℃ for heat treatment for 30 min;
6) uniformly mixing a coupling agent and acetone with the mass 90 times that of the coupling agent;
7) stirring and dispersing the aramid fiber pulp obtained in the step 5) in the coupling agent dilute solution obtained in the step 6);
8) standing the mixed solution obtained in the step 7) for 12 hours;
9) after the modified aramid pulp obtained in the step 8) is desolventized, the modified aramid pulp is placed in an environment with the temperature of 120 ℃ for heat treatment for 30 min;
10) adding a separant into the modified aramid pulp obtained in the step 9), and uniformly mixing to obtain the aramid pulp dispersion.
Example 2
An aramid pulp dispersion and a preparation method thereof, the specific steps are as follows:
1) weighing 20 parts of aramid pulp, 2 parts of hexamethylene diisocyanate serving as a modifier, KH-5503 parts of silane coupling agent and 5 parts of white carbon black serving as a separant; weighing 200 parts of a dispersion solvent n-hexane;
2) uniformly mixing the modifier with acetone with the mass 40 times that of the modifier;
3) stirring and dispersing aramid pulp in the modifier dilute solution obtained in the step 2);
4) standing the mixed solution obtained in the step 3) for 10 hours;
5) removing the solvent from the modified aramid pulp mixed solution obtained in the step 4) by adopting a negative pressure suction filtration mode, and then placing the mixture in an environment with the temperature of 80 ℃ for heat treatment for 60 min;
6) uniformly mixing a coupling agent and acetone with the mass 40 times that of the coupling agent;
7) stirring and dispersing the aramid fiber pulp obtained in the step 5) in the coupling agent dilute solution obtained in the step 6);
8) standing the mixed solution obtained in the step 7) for 15 hours;
9) after the modified aramid pulp obtained in the step 8) is desolventized, the modified aramid pulp is placed in an environment with the temperature of 100 ℃ for heat treatment for 30 min;
10) adding a separant into the modified aramid pulp obtained in the step 9), and uniformly mixing to obtain the aramid pulp dispersion.
Example 3
An aramid pulp dispersion and a preparation method thereof, the specific steps are as follows:
1) weighing 10 parts of aramid pulp, 2 parts of toluene diisocyanate serving as a modifier, KH-5802 parts of silane coupling agent and 10 parts of carbon black serving as a separant; weighing 200 parts of dispersion solvent cyclohexane;
2) uniformly mixing a modifier with acetone with the mass 50 times that of the modifier;
3) stirring and dispersing aramid pulp in the modifier dilute solution obtained in the step 2);
4) standing the mixed solution obtained in the step 3) for 24 hours;
5) removing the solvent from the modified aramid pulp mixed solution obtained in the step 4), and then, placing the mixture in an environment with the temperature of 100 ℃ for heat treatment for 40 min;
6) uniformly mixing a coupling agent and acetone with the mass 50 times that of the coupling agent;
7) stirring and dispersing the aramid fiber pulp obtained in the step 5) in the coupling agent dilute solution obtained in the step 6);
8) standing the mixed solution obtained in the step 7) for 20 hours;
9) after the modified aramid pulp obtained in the step 8) is desolventized, the modified aramid pulp is placed in an environment with the temperature of 100 ℃ for heat treatment for 40 min;
10) adding a separant into the modified aramid pulp obtained in the step 9), and uniformly mixing to obtain the aramid pulp dispersion.
Examples of the experiments
An experiment was performed using the aramid pulp dispersion prepared in example 1.
1 part of aramid pulp dispersion and aramid pulp elastomer of DuPont are respectively added into a natural rubber formula (the formula is shown in table 1), the influence of the aramid pulp dispersion and the aramid pulp elastomer of DuPont on the fatigue life of the material is researched, meanwhile, a blank control group is set, and aramid pulp is not added into the control group.
TABLE 1 Experimental examples Natural rubber formulations
The sample preparation process is as follows:
1) first-stage mixing: adding raw rubber into an internal mixer for internal mixing for 2min, adding compounding agents except carbon black and aramid pulp for internal mixing for 4min, then adding carbon black and aramid pulp dispersion or elastomer for internal mixing for 4min, discharging rubber, discharging sheets and standing for 24 h;
2) and (3) second-stage mixing: adding sulfur and accelerator into the first-stage glue on an open mill, thinly passing for 15 times, rolling for 3 times, discharging, and standing for 24 h;
3) and (3) vulcanization molding: and pressing the rubber compound after the placement on a vacuum vulcanizing machine to obtain a test piece.
Testing the fatigue life of the material according to GB/T1688-.
Tests show that the fatigue life of the natural rubber without the aramid pulp is 17 ten thousand times, and the fatigue life of the natural rubber with the aramid pulp dispersion and the aramid pulp elastomer which are added in equal amounts is 24 ten thousand times and 13 ten thousand times respectively. The fatigue life of the former is obviously increased by 41%; in the latter, the material dispersibility is emphasized, and the interface strength is not considered, which is equivalent to introducing a defect source into the matrix, so that the fatigue life is reduced.
Meanwhile, the addition amount of the used modified aramid pulp is small, the processing performance of the base material is not influenced, and the tearing strength of the material can be improved by more than 25% by only adding 1 part of aramid pulp.
Claims (4)
1. An aramid pulp dispersion, characterized in that: the main components are as follows by weight:
10-20 parts of aramid pulp, 2-4 parts of modifier and 2-4 parts of coupling agent
5-20 parts of a release agent;
wherein the modifier is one of toluene diisocyanate, hexamethylene diisocyanate and diphenylmethane diisocyanate;
the coupling agent is a silane coupling agent;
the separant is calcium carbonate or talcum powder or carbon black or white carbon black;
the preparation method comprises the following process steps:
1) uniformly mixing the modifier with the formula amount and a dispersion solvent with the mass 20-100 times of that of the modifier;
2) stirring and dispersing aramid fiber pulp with a formula amount in the modifier dilute solution obtained in the step 1);
3) standing the mixed solution obtained in the step 2) for 10-30 h;
4) removing the solvent from the modified aramid pulp mixed solution obtained in the step 3), and then, placing the mixture in an environment with the temperature of 80-120 ℃ for heat treatment for 20-90 min;
5) uniformly mixing the coupling agent with the formula amount and a dispersion solvent with the mass 20-100 times of that of the coupling agent;
6) stirring and dispersing the aramid pulp obtained in the step 4) in the coupling agent dilute solution obtained in the step 5);
7) standing the mixed solution obtained in the step 6) for 10-30 h;
8) after the modified aramid pulp obtained in the step 7) is desolventized, placing the modified aramid pulp in an environment with the temperature of 80-120 ℃ and carrying out heat treatment for 20-90 min;
9) adding a formula amount of separant into the modified aramid pulp obtained in the step 8), and uniformly mixing to obtain an aramid pulp dispersion;
the dispersing solvent adopted in the steps 1) and 5) is acetone or alkane solvent.
2. The aramid pulp dispersion as claimed in claim 1, characterized in that: the coupling agent is one of KH-602, KH-590, KH-580, KH-570, KH-560 and KH-550.
3. The process for producing the aramid pulp dispersion as claimed in claim 1, characterized in that: the method comprises the following process steps:
1) uniformly mixing the modifier with the formula amount and a dispersion solvent with the mass 20-100 times of that of the modifier;
2) stirring and dispersing aramid fiber pulp with a formula amount in the modifier dilute solution obtained in the step 1);
3) standing the mixed solution obtained in the step 2) for 10-30 h;
4) removing the solvent from the modified aramid pulp mixed solution obtained in the step 3), and then, placing the mixture in an environment with the temperature of 80-120 ℃ for heat treatment for 20-90 min;
5) uniformly mixing the coupling agent with the formula amount and a dispersion solvent with the mass 20-100 times of that of the coupling agent;
6) stirring and dispersing the aramid pulp obtained in the step 4) in the coupling agent dilute solution obtained in the step 5);
7) standing the mixed solution obtained in the step 6) for 10-30 h;
8) after the modified aramid pulp obtained in the step 7) is desolventized, placing the modified aramid pulp in an environment with the temperature of 80-120 ℃ and carrying out heat treatment for 20-90 min;
9) adding a formula amount of separant into the modified aramid pulp obtained in the step 8), and uniformly mixing to obtain an aramid pulp dispersion;
the dispersing solvent adopted in the steps 1) and 5) is acetone or alkane solvent.
4. The method for producing an aramid pulp dispersion as claimed in claim 3, characterized in that:
and 4) performing negative pressure suction filtration or centrifugal drying on the desolventizing agent in the steps 4) and 7).
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| CN115536850A (en) * | 2021-06-14 | 2022-12-30 | 南京科技职业学院 | Aramid pulp modification method, reinforced rubber composite material and preparation method |
| CN113354879B (en) * | 2021-06-16 | 2023-01-24 | 山东非金属材料研究所 | Vibration damping rubber and preparation method thereof |
| CN115558291A (en) * | 2021-07-03 | 2023-01-03 | 南京科技职业学院 | Preparation method of flaky white carbon black modified aramid pulp |
| CN117362876A (en) * | 2022-06-10 | 2024-01-09 | 辽宁天源大奔科技集团有限公司 | Aramid pulp reinforced PVC-C mine sleeve and preparation method thereof |
| CN117051591B (en) * | 2023-10-12 | 2024-08-09 | 烟台泰和兴材料科技股份有限公司 | Aramid pulp modification treatment method, aramid pulp pre-dispersion and application thereof |
Citations (3)
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|---|---|---|---|---|
| EP2101079A2 (en) * | 2008-03-11 | 2009-09-16 | ContiTech Antriebssysteme GmbH | Belt, in particular power transmission belt, with a coating with a polyisocyanurate-polyuric material as adhesive and method for its production |
| CN102134394A (en) * | 2011-01-07 | 2011-07-27 | 杭州顺隆胶辊有限公司 | Aramid fiber pulp dispersion and preparation method thereof |
| CN108103769A (en) * | 2018-01-16 | 2018-06-01 | 烟台泰和工程材料有限公司 | A kind of aramid fiber surface treatment fluid and preparation method thereof |
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| US20070149656A1 (en) * | 2005-12-23 | 2007-06-28 | 3M Innovative Properties Company | Sprayable mining liner composition |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2101079A2 (en) * | 2008-03-11 | 2009-09-16 | ContiTech Antriebssysteme GmbH | Belt, in particular power transmission belt, with a coating with a polyisocyanurate-polyuric material as adhesive and method for its production |
| CN102134394A (en) * | 2011-01-07 | 2011-07-27 | 杭州顺隆胶辊有限公司 | Aramid fiber pulp dispersion and preparation method thereof |
| CN108103769A (en) * | 2018-01-16 | 2018-06-01 | 烟台泰和工程材料有限公司 | A kind of aramid fiber surface treatment fluid and preparation method thereof |
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