CN109957966A - A kind of aramid fiber surface modified method - Google Patents
A kind of aramid fiber surface modified method Download PDFInfo
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- CN109957966A CN109957966A CN201910212113.0A CN201910212113A CN109957966A CN 109957966 A CN109957966 A CN 109957966A CN 201910212113 A CN201910212113 A CN 201910212113A CN 109957966 A CN109957966 A CN 109957966A
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- aramid fiber
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- isocyanates
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/395—Isocyanates
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention provides a kind of aramid fiber surface modified method comprising following step: S1: being impregnated aramid fiber 1~3 hour at a temperature of 50~15 DEG C with isocyanates, cleans drying；S2: the acetone soln for the epoxy resin for being again 6~18% with mass percent concentration impregnates aramid fiber 2.5~4 hours at normal temperature, completes after drying modified to the surface of aramid fiber.The present inventor is for many years on the basis of polyester fibre surface pre-processes production and exploitation, fiber surface activating pretreatment is technically improved, innovation transformation more is carried out in the RFL tackified finish formula and process aspect of the second bath, the bonding enhancing that can meet different matrix requires；The proportion of a bath maceration extract and the technological parameter of impregnation of the invention have passed through and test repeatedly, it is determined that specific parameter has reached optimum efficiency.
Description
Technical field
The present invention relates to aramid fiber technical field of modification, specially a kind of aramid fiber surface modified method.
Background technique
Aramid fiber is one of ideal framework material, since it is with the very high degree of orientation and cleanliness, and is not had
Amorphous region, and have a large amount of phenyl ring in molecule segment, steric hindrance is larger, therefore amide group is more difficult occurs with other atoms or group
Chemical reaction, so it is relatively difficult to carry out bonding impregnation for aramid fiber surface.Based on this domestic and international experts and scholars couple
The surface bonding modification of aramid fiber has conducted extensive research and tests, compound into aramid fiber/rubber of industrial applications at present
The aramid fiber surface of material is handled frequently at the surface for using coupling agent after latex, plasma, phosphoric acid corrosion fiber surface
Reason method achieves certain effect, but mainly improves the interfacial bonding of base rubber material and aramid fiber in a manner of physics, because
This interfacial adhesion strength has the space further increased.The dispersion of fiber is then the another technical problem of industry, if making fiber
Be uniformly dispersed and be excessively kneaded, will lead to fibre length excessively reduce, molecular weight rubber decline, deteriorate performance；If fiber is long
Degree is long but disperses the composite material that unevenness equally also cannot get function admirable.Inventor by locating in polyester fibre surface in advance for many years
On the basis of reason production and exploitation, fiber surface activating pretreatment is technically improved, different rubber matrixs can be met
Bonding requires.
Summary of the invention
The purpose of the present invention is to provide a kind of aramid fiber surface modified methods, to solve to propose in above-mentioned background technique
The problem of.
To achieve the above object, the invention provides the following technical scheme:
A kind of aramid fiber surface modified method comprising following step:
S1: being impregnated aramid fiber 1~3 hour at a temperature of 50~15 DEG C with isocyanates, cleans drying；
S2: the acetone soln for the epoxy resin for being again 6~18% with mass percent concentration impregnates aramid fiber fibre at normal temperature
Dimension 2.5~4 hours completes modified to the surface of aramid fiber after drying.
Further, the isocyanates selects the closed polyisocyanates of phenol.
Further, the closed polyisocyanates of the phenol selects Desmodur AP stable hard resin, this this it is solid
Body resin is dissolved in ethyl acetate, propylene glycol monomethyl ether acetate, methyl ethyl ketone and alcohols solvent, can use dimethylbenzene, solvent naphtha
Adjust viscosity.
Further, the drying temperature after the isocyanates dipping aramid fiber is 230 DEG C, and drying time is 3 hours.
Further, the drying temperature after the epoxy resin acetone soln dipping aramid fiber is 85 DEG C, and the time is small for 2.5
When.
Further, the isocyanates is first at normal temperature with ultrasonic cleaning aramid fiber 2 hours or more before impregnating aramid fiber, then
It is dried 1.5 hours at 120 DEG C, makes it dry and remove the organic coating of its surface attachment.
In conclusion the invention has the following advantages:
The present inventor is for many years on the basis of polyester fibre surface pre-processes production and exploitation, using first activating again
The two-bath process impregnation technology of RFL thickening not only improves in the fiber surface activating pretreatment technology of a bath, more exists
The RFL tackified finish formula and process aspect of second bath have carried out innovation transformation, and the bonding enhancing that can meet different matrix requires；
The present invention one bathes maceration extract, two bath RF resins, the proportion of RFL maceration extract and the technological parameter of impregnation and have passed through instead
Multiple experiment, it is determined that specific parameter has reached optimum efficiency.
Detailed description of the invention
Fig. 1 is that isocyanates of the invention and aramid fiber react schematic diagram.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
There are a large amount of phenyl ring in aramid fiber molecule segment, steric hindrance is larger, therefore amide group is more difficult with other atoms or base
Group chemically reacts, so it is relatively difficult to carry out bonding impregnation for aramid fiber surface.RF resin is a kind of space
The polymer of structure is not linear structure.By taking rubber as an example, after impregnation, we carry out heat cure processing, and RF resin can be with
Hydrogen bond connection etc. is established in latex surface reaction, and therefore, the molecule of RF resin volumes structure can combine closely with latex, will be each
The entirety that a latex particle links together as a space structure.Each latex particle is mutual by RF resin in other words
It links together.RF resin be in entire adhesion process latex particle is established between each other closely combination, while and
Aramid fiber, which is established, to be combined.But after RF resin completes heat cure in immersing glue process, the phenolic resin in rubber shoe latex layer is
Activity is lost, without further respond.
Therefore the important function of RF is that latex particle and aramid fiber bonding, while latex particle also mutually being interconnected
It is connected together.Aramid fiber impregnation is exactly that latex particle in dipping solution and aramid fiber are bonded together, while also mutually gluing
It is combined.It must have the group with RF resin reaction in aramid fiber, and aramid fiber does not have this active group, it is necessary to it carries out
A kind of aramid fiber surface modified method through the invention is activated.
The present invention is implemented by following scheme:
The isocyanates is first used ultrasonic cleaning aramid fiber 2 hours or more at normal temperature before impregnating aramid fiber, then at 120 DEG C
It is lower to dry 1.5 hours, make it dry and remove the organic coating of its surface attachment.Then,
S1: being impregnated aramid fiber 1~3 hour at a temperature of 50~15 DEG C with isocyanates, cleans drying；The isocyanic acid
Drying temperature after ester dipping aramid fiber is 230 DEG C, and drying time is 3 hours.
Reaction process is as shown in Figure 1, two kinds of substances that isocyanates and aramid fiber reaction generate, remaining isocyanate function
Group can also further react with subsequent RFL rubber shoe latex layer.
S2: the acetone soln for the epoxy resin for being again 6~18% with mass percent concentration impregnates aramid fiber fibre at normal temperature
Dimension 2.5~4 hours completes modified to the surface of aramid fiber after drying.
In one preferred scheme, the isocyanates selects the closed polyisocyanates of phenol.The phenol is closed
Polyisocyanates selects Desmodur AP stable hard resin, which is dissolved in ethyl acetate, propylene glycol list first
Ether acetate, methyl ethyl ketone and alcohols solvent can adjust viscosity with dimethylbenzene, solvent naphtha.The epoxy resin acetone soln
Impregnate aramid fiber after drying temperature be 85 DEG C, the time be 2.5 hours.
Experimental example 1:
Aramid filament (trade mark: AF-1000,1500 denier, ALKEX company, South Korea) is cut into 20mm sections, it is clear with acetone ultrasound
It is dried after washing aramid fiber 1 hour, removes the organic coating of its surface attachment；
S1: it by the smooth releasing of aramid fiber precursor pay off rack, keeps not loose, not upper and twists；
S2: being combed by separated time and reach first group of drawing-off rod, is entered the first glue groove by deflector roll and is carried out a bath；Benzene is selected in one bath
The polyisocyanates of phenol block, specifically includes step 1: aramid fiber 1~3 is impregnated at a temperature of 50~15 DEG C with isocyanates
Hour, clean drying；Step 2: the acetone soln for the epoxy resin for being again 6~18% with mass percent concentration is at normal temperature
Dipping aramid fiber 2.5~4 hours completes modified to the surface of aramid fiber after drying.
S3: entering first layer baking oven and dry, and drying temperature is 105 DEG C, and drying time is 3 hours；
S4: enter second layer baking oven by second group of draw roll and carry out 230 DEG C of hot settings；
S5: and then enter the second glue groove by third group draw roll and carry out two baths；With traditional RFL dipping solution in 19 DEG C of temperature
Lower dipping aramid fiber 3.2 hours；
S6: it is dried by third layer；Drying temperature be 85 DEG C, the time be 2.5 hours；
S7: up- coiler molding is sent to by the 4th group of draw roll after the 4th layer of pyroreaction of progress and is made into aramid fiber silk.
Experimental example 2:
Under same experimental conditions, the step S1-S8 of comparative experiments example 1 does not carry out any processing.
Comparative experiments:
40 grams of aramid fiber short fibre are weighed obtained in experimental example 1,2,3 respectively, are equipped with 1000 grams of natural rubbers, 17 grams of sulphur
Vulcanizing agent and 10 grams of compounding agents；Compounding agent includes 30 grams of zinc oxide, 20 grams of stearic acid, 17.1 grams of captaxes, 14.7 grams of promotors
DM, 5 grams of diphenylguanidines, 3.2 grams of Vulcanization accelerator TMTDs and 10 grams of antioxidant SP-C.
They are kneaded 10 minutes in mixer at 120 DEG C, revolving speed 80r/min, then the double roller at 60 DEG C is opened
It is kneaded in mill, 17g sulfur vulcanizing agent and 100g compounding agent is added, Bao Tong 4 times, obtains rubber compound；By rubber compound at 145 DEG C
According to the sulfurizing time tc90 vulcanization of vulcameter measurement, modifying aramid fiber and sulfurized natural rubber composite material are prepared.
Table 1 is by two-bath process of the present invention, mono bath dipping process, the native rubber composite material performance pair for not being modified processing
Than
Show the mechanical property of the aramid fiber enhancing rubber composite material of the technology of the present invention preparation according to the test result of table 1
It is better than mono bath dipping process and is not modified the rubber composite material of processing, the aramid fiber of the technology of the present invention preparation enhances rubber
Composite material has a clear superiority.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
Claims (6)
1. a kind of aramid fiber surface modified method, which is characterized in that it is comprised the following steps that
S1: being impregnated aramid fiber 1~3 hour at a temperature of 50~15 DEG C with isocyanates, cleans drying；
S2: the acetone soln for the epoxy resin for being again 6~18% with mass percent concentration impregnates aramid fiber 2.5 at normal temperature
It~4 hours, is completed after drying modified to the surface of aramid fiber.
2. a kind of aramid fiber surface modified method according to claim 1, it is characterised in that: the isocyanates is selected
The closed polyisocyanates of phenol.
3. a kind of aramid fiber surface modified method according to claim 1, it is characterised in that: the phenol is closed more
Isocyanates selects Desmodur AP stable hard resin, which is dissolved in ethyl acetate, propylene glycol monomethyl ether
Acetate, methyl ethyl ketone and alcohols solvent can adjust viscosity with dimethylbenzene, solvent naphtha.
4. a kind of aramid fiber surface modified method according to claim 1, it is characterised in that: the isocyanates dipping
Drying temperature after aramid fiber is 105 DEG C, and drying time is 3 hours.
5. a kind of aramid fiber surface modified method according to claim 1, it is characterised in that: the epoxy resin acetone
Solution impregnate aramid fiber after drying temperature be 85 DEG C, the time be 2.5 hours.
6. a kind of aramid fiber surface modified method according to claim 1, it is characterised in that: the isocyanates is soaking
It is first then dried 1.5 hours at 120 DEG C at normal temperature with ultrasonic cleaning aramid fiber 2 hours or more before stain aramid fiber, makes it dry and remove
The organic coating for going to its surface to adhere to.
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Cited By (3)
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| CN110863297A (en) * | 2019-11-12 | 2020-03-06 | 广州中樱汽车零部件有限公司 | Environment-friendly recycled material low-VOC (volatile organic compound) hybrid cotton for automobiles and preparation method thereof |
| CN113463396A (en) * | 2021-07-01 | 2021-10-01 | 黑龙江弘宇短纤维新材料股份有限公司 | Aramid short fiber for nylon resin product and preparation method thereof |
| CN116065387A (en) * | 2023-02-20 | 2023-05-05 | 黑龙江弘宇短纤维新材料股份有限公司 | Aramid fiber wire and preparation method and application thereof |
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| CN116065387A (en) * | 2023-02-20 | 2023-05-05 | 黑龙江弘宇短纤维新材料股份有限公司 | Aramid fiber wire and preparation method and application thereof |
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