CN110078952A - A kind of preparation method of aramid fiber carbon fiber composite reinforced material - Google Patents
A kind of preparation method of aramid fiber carbon fiber composite reinforced material Download PDFInfo
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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
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/042—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with carbon fibres
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- 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
- C08J5/046—Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/047—Reinforcing macromolecular compounds with loose or coherent fibrous material with mixed 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
- 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
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Abstract
The present invention provides a kind of preparation method of aramid fiber carbon fiber composite reinforced material, it includes the following steps: to be made by resin, aramid fiber short fibre film and carbon fibre fabric, and dipping modification has been carried out to aramid fiber short fibre film, treatment process is as follows: A: one bath；B: it dries for the first time；C: two baths；D: secondary drying；Wherein: pre- impregnation being carried out using the isocyanates that the high activity of aqueous solution type is reacted in the step A；It is impregnated in step C using RFL maceration extract.The present invention is not only improved in the fiber surface activating pretreatment technology of a bath using the two-bath process impregnation technology for first activating again RFL thickening, has more carried out innovation transformation in the RFL tackified finish formula and process aspect of the second bath.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 and test repeatedly, it is determined that specific parameter has reached optimum efficiency.
Description
Technical field
The present invention relates to aramid fiber preparation technical field, specially a kind of preparation of aramid fiber carbon fiber composite reinforced material
Method.
Background technique
The advantages that for carbon fiber sandwich structure with its lightweight, specific strength is high, and specific modulus is high, heat-insulated, sound insulation, corrosion-resistant is extensive
Applied to aerospace, shipping industry, automobile manufacture, the various fields such as style leisure equipment, along with carbon fibre composite
Extensive use, however the popularization of carbon fibre reinforced composite it is poor by shock resistance, easily layering, the easy unsticking in face core interface
The disadvantages of restriction, for improve composite material interface toughness, propose a variety of improved technologies.
Impregnation aramid fiber short fibre can be used as the preferred material to solve the above problems and be distributed in component carbon fibers, improve carbon fiber
The performance of dimension.But due to aramid fiber its with the very high degree of orientation and cleanliness, and there is no amorphous region, and molecule
There are a large amount of phenyl ring in segment, steric hindrance is larger, therefore amide group is more difficult chemically reacts with other atoms or group, so right
It is relatively difficult that bonding impregnation is carried out in aramid fiber surface, it is bad for improving the compound carbon fibre material impact of performance.
Summary of the invention
A kind of preparation method of aramid fiber carbon fiber composite reinforced material, to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of aramid fiber carbon fiber composite reinforced material, by resin, aramid fiber short fibre film
It is made with carbon fibre fabric, the specific steps are as follows:
(1) aramid fabric cutting, stirring, laying are formed into the aramid fiber short fibre film with certain surface density, and
Processing is modified to aramid fiber short fibre film；
(2) by resin thorough impregnation carbon fibre fabric and aramid fiber short fibre film；
(3) cover aramid fiber short fibre film commonly through pressing device carbon fibre fabric and aramid fiber short fibre film
Reinforcing material is made into carbon fibre fabric surface layer；
Wherein, specific step is as follows for modification in step (1):
Wherein, specific step is as follows in step 1:
A: one bath；
B: it dries for the first time；
C: two baths；
D: secondary drying；
Wherein:
Pre- impregnation is carried out using the isocyanates that the high activity of aqueous solution type is reacted in the step A；
It is impregnated in step C using RFL maceration extract, the formula of the RFL maceration extract is:
RF resin: 420.6 parts of parts by weight；
Soft water: 95.2 parts of parts by weight；
VP latex 40%: 484.2 parts of parts by weight；
The wherein formula of RF resin are as follows:
Soft water: 425.6 parts of parts by weight；
Sodium hydroxide 7%: 16 parts of parts by weight；
Resorcinol solid: 22 parts of parts by weight；
Formaldehyde 38%: 13 parts of parts by weight；
Its specific work step includes:
S1: aramid fiber short fibre film is subjected to ultrasonic removal of impurities；
S2: enter the first glue groove and carry out a bath；
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 RFL dipping solution obtained in 19 DEG C of temperature
Degree 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: the 4th layer of pyroreaction is carried out；
Wherein, in the step S2, the closed polyisocyanates of phenol is selected in a bath, specifically
Step 1: being impregnated aramid fiber 1~3 hour at a temperature of 50~15 DEG C with isocyanates, cleans drying；
Step 2: the acetone soln for the epoxy resin for being again 6~18% with mass percent concentration impregnates virtue at normal temperature
It synthetic fibre fiber 2.5~4 hours, is completed after drying modified to the surface of aramid fiber.
Further, specific as follows in the step S5:
One, prepare 420.6 parts of parts by weight of RF resin liquid, 95.2 parts of parts by weight of soft water and 484.2 parts of parts by weight of VP
Latex 40%, total weight parts 1000；
Two, soft water and VP latex are put into blend tank；
Three, RF resin liquid is transplanted in blend tank, and continues to stir, transfer RF resin liquid is completed in 10 minutes, RF
Resin liquid uses the transfer mode of fountain, and blend tank, which is adopted, is water-cooled jacket heat-preservation, keeps the glue temperature 20 in blend tank
DEG C, pH value is adjusted between 8-9；
Four, since the transfer of RF resin, after curing in 27 hours, obtained RFL maceration extract is sent into subsequent cement dipping machine
It uses.
The preparation method of RF resin liquid therein, comprising the following steps:
(1) prepare the formaldehyde 38% of soft water, 22 parts of parts by weight of resorcinol solid and parts by weight 13；
(2) soft water is put into reactor tank, water temperature is controlled at 23 DEG C；
(3) sodium hydroxide is dissolved in soft water, is launched after being configured to the sodium hydrate aqueous solution that concentration is 7% to reaction
In tank, sodium hydrate aqueous solution parts by weight are 16 parts, and are stirred 10 minutes；
(4) resorcinol solid is dissolved in soft water, is launched after being configured to the resorcinol solution of concentration 10~20%
Into reactor tank, and it is stirred 20 minutes；
(5) formaldehyde 38% is launched into soft water and is mixed, the formalin that concentration is 5~20% is configured to, by formaldehyde
Aqueous solution is slowly added in reactor tank, and continues stirred tank；
(6) with 10 DEG C of temperature of the cooling reactor tank of cooling water, control reaction temperature is 20 DEG C, and the reaction time is 12.5 small
When, obtain RF resin liquid.
In conclusion the invention has the following advantages:
Inventor has carried out modification to aramid fiber film, at the two-bath process dipping for first activating again RFL thickening
Reason technology not only improves in the fiber surface activating pretreatment technology of a bath, more matches in the RFL tackified finish of the second bath
Side and process aspect have carried out innovation transformation, and the bonding enhancing that can meet carbon fibrous body requires.
It is equal that the present invention one bathes maceration extract, two bath RF resins, the proportion of RFL maceration extract and the technological parameter of impregnation
It has passed through and test repeatedly, it is determined that specific parameter has reached optimum efficiency, shock resistance and Mian Xin circle is greatly improved
Face adhesive property.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
A kind of preparation method of aramid fiber carbon fiber composite reinforced material, by resin, aramid fiber short fibre film and carbon fiber
Fabric is made, the specific steps are as follows:
(1) aramid fabric cutting, stirring, laying are formed into the aramid fiber short fibre film with certain surface density, and
Processing is modified to aramid fiber short fibre film；
(2) by resin thorough impregnation carbon fibre fabric and aramid fiber short fibre film；
(3) cover aramid fiber short fibre film commonly through pressing device carbon fibre fabric and aramid fiber short fibre film
Reinforcing material is made into carbon fibre fabric surface layer；
Wherein, specific step is as follows for modification in step (1):
Wherein, specific step is as follows in step 1:
It includes that following processing step is carried out to aramid fiber precursor: A: one bath；B: it dries for the first time；C: two baths；D: secondary baking
It is dry；E: winding；F: cutting；Wherein: being presoaked in the step A using the isocyanates that the high activity of aqueous solution type is reacted
Glue；It is impregnated in step C using RFL maceration extract, the formula of the RFL maceration extract is: RF resin: 420.6 parts of parts by weight；It is soft
Water: 95.2 parts of parts by weight；VP latex 40%: 484.2 parts of parts by weight；The wherein formula of RF resin are as follows: soft water: parts by weight 425.6
Part；Sodium hydroxide 7%: 16 parts of parts by weight；Resorcinol solid: 22 parts of parts by weight；Formaldehyde 38%: 13 parts of parts by weight；
Its specific work step includes:
S1: aramid fiber short fibre film is subjected to ultrasonic removal of impurities；
S2: enter the first glue groove and carry out a bath；The closed polyisocyanates of phenol is selected in one bath, specifically includes step 1:
It is impregnated aramid fiber 1~3 hour at a temperature of 50~15 DEG C with isocyanates, cleans drying；Step 2: mass percent is used again
The acetone soln for the epoxy resin that concentration is 6~18% impregnates aramid fiber 2.5~4 hours at normal temperature, completes after drying
It is modified to the surface of aramid fiber.
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 RFL dipping solution obtained in 19 DEG C of temperature
Degree 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 semi-finished product；
S8: finished product is made into after semi-finished product are cut off using fibre cutting machine.
The allotment of embodiment 1:RF resin liquid；
(1) prepare the formaldehyde 38% of soft water, 22 parts of parts by weight of resorcinol solid and parts by weight 13；
(2) soft water is put into reactor tank, water temperature is controlled at 23 DEG C；
(3) sodium hydroxide is dissolved in soft water, is launched after being configured to the sodium hydrate aqueous solution that concentration is 7% to reaction
In tank, sodium hydrate aqueous solution parts by weight are 16 parts, and are stirred 10 minutes；
(4) resorcinol solid is dissolved in soft water, is launched after being configured to the resorcinol solution of concentration 10~20%
Into reactor tank, and it is stirred 20 minutes；
(5) formaldehyde 38% is launched into soft water and is mixed, the formalin that concentration is 5~20% is configured to, by formaldehyde
Aqueous solution is slowly added in reactor tank, and continues stirred tank；
(6) with 10 DEG C of temperature of the cooling reactor tank of cooling water, control reaction temperature is 20 DEG C, and the reaction time is 12.5 small
When, obtain RF resin liquid.
The allotment of embodiment 2:RFL maceration extract；
One, prepare 420.6 parts of parts by weight of RF resin liquid, 95.2 parts of parts by weight of soft water and 484.2 parts of parts by weight of VP
Latex 40%, total weight parts 1000；
Two, soft water and VP latex are put into blend tank；
Three, RF resin liquid is transplanted in blend tank, and continues to stir, transfer RF resin liquid is completed in 10 minutes, RF
Resin liquid uses the transfer mode of fountain, and blend tank, which is adopted, is water-cooled jacket heat-preservation, keeps the glue temperature 20 in blend tank
DEG C, pH value is adjusted between 8-9；
Four, since the transfer of RF resin, after curing in 27 hours, obtained RFL maceration extract is sent into subsequent cement dipping machine
It uses.
Experimental example 1:
By aramid fabric cutting, stirring, it is laid with the aramid fiber short fibre film for being formed and there is certain surface density, and to virtue
Synthetic fibre staple fiber film is modified processing；
S1: aramid fiber short fibre film is subjected to ultrasonic removal of impurities；
S2: enter the first glue groove and carry out a bath；The closed polyisocyanates of phenol is selected in one bath, specifically includes step 1:
It is impregnated aramid fiber 1~3 hour at a temperature of 50~15 DEG C with isocyanates, cleans drying；Step 2: mass percent is used again
The acetone soln for the epoxy resin that concentration is 6~18% impregnates aramid fiber 2.5~4 hours at normal temperature, completes after drying
It is modified to the surface of aramid fiber.
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；Made from embodiment 1 and embodiment 2
RFL dipping solution impregnates aramid fiber 3.2 hours at a temperature of 19 DEG C；
S6: it is dried by third layer；Drying temperature be 85 DEG C, the time be 2.5 hours；
S7: the 4th layer of pyroreaction is carried out.
Experimental example 2:
Under same experimental conditions, the step S1-S8 of comparative experiments example 1, step is changed to produce using Changzhou Shuguang Chemical Factory
" Vulkabond E " RP mono bath impregnation, it is the contracting of a kind of parachlorophenol being dissolved in ammonium hydroxide, formaldehyde and resorcinol
Polymers impregnates at a temperature of 19 DEG C aramid fiber 3.2 hours, and baking and curing processing is then carried out at 240 DEG C of temperature and is completed.
Experimental example 3:
Under same experimental conditions, the step S1-S8 of comparative experiments example 1 does not carry out any processing.
Comparative experiments:
Take carbon fibre fabric and experimental example 1,2,3 treated aramid fiber short fibre film
By resin thorough impregnation carbon fibre fabric and aramid fiber short fibre film；
By carbon fibre fabric and aramid fiber short fibre film commonly through pressing device, cover aramid fiber short fibre film in carbon
Reinforcing material is made into fabric surface layer.
Table 1 presses the carbon fibre composite performance comparison of experimental example 1,2,3 of the present invention processing
Show that the mechanical property of the carbon fiber of the technology of the present invention preparation is better than at mono bath impregnation according to the test result of table 1
Reason and the carbon fibre composite for not being modified processing, the carbon fibre composite of the technology of the present invention preparation have obvious excellent
Gesture.
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 label in claim should not be construed as limiting the claims involved.
Claims (4)
1. a kind of preparation method of aramid fiber carbon fiber composite reinforced material, which is characterized in that it is by resin, aramid fiber short fibre film
It is made with carbon fibre fabric, the specific steps are as follows:
By aramid fabric cutting, stirring, it is laid with the aramid fiber short fibre film for being formed and there is certain surface density, and short to aramid fiber
Fiber membrane is modified processing；
By resin thorough impregnation carbon fibre fabric and aramid fiber short fibre film；
By carbon fibre fabric and aramid fiber short fibre film commonly through pressing device, cover aramid fiber short fibre film in carbon fiber
Reinforcing material is made into textile surface；
Wherein, specific step is as follows for modification in step (1):
A: one bath；B: it dries for the first time；C: two baths；D: secondary drying；
Wherein:
Pre- impregnation is carried out using the isocyanates that the high activity of aqueous solution type is reacted in the step A；It is soaked in step C using RFL
Stain liquid is impregnated, and the formula of the RFL maceration extract is: RF resin: 420.6 parts of parts by weight；Soft water: 95.2 parts of parts by weight；VP
Latex 40%: 484.2 parts of parts by weight；The wherein formula of RF resin are as follows: soft water: 425.6 parts of parts by weight；Sodium hydroxide 7%: weight
16 parts of part；Resorcinol solid: 22 parts of parts by weight；Formaldehyde 38%: 13 parts of parts by weight；Its specific work step includes:
S1: aramid fiber short fibre film is subjected to ultrasonic removal of impurities；
S2: enter the first glue groove and carry out a bath；
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 RFL dipping solution obtained at a temperature of 19 DEG C
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: it carries out the 4th layer of pyroreaction post-processing and completes.
2. a kind of preparation method of aramid fiber carbon fiber composite reinforced material according to claim 1, it is characterised in that: described
In step S2, the closed polyisocyanates of phenol is selected in a bath, specific:
Step 1: being impregnated aramid fiber 1~3 hour at a temperature of 50~15 DEG C with isocyanates, cleans drying；
Step 2: the acetone soln for the epoxy resin for being again 6~18% with mass percent concentration impregnates aramid fiber at normal temperature
It 2.5~4 hours, is completed after drying modified to the surface of aramid fiber.
3. a kind of preparation method of aramid fiber carbon fiber composite reinforced material according to claim 1, it is characterised in that: described
It is specific as follows in step S5:
One, prepare 420.6 parts of parts by weight of RF resin liquid, 95.2 parts of parts by weight of soft water and 484.2 parts of parts by weight of VP latex
40%, total weight parts 1000；
Two, soft water and VP latex are put into blend tank；
Three, RF resin liquid is transplanted in blend tank, and continues to stir, transfer RF resin liquid is completed in 10 minutes, RF resin
Liquid uses the transfer mode of fountain, and blend tank, which is adopted, is water-cooled jacket heat-preservation, keeps 20 DEG C of glue temperature in blend tank, PH
Value is adjusted between 8-9；
Four, since the transfer of RF resin, after curing in 27 hours, obtained RFL maceration extract is sent into subsequent cement dipping machine and is used.
4. a kind of preparation method of aramid fiber carbon fiber composite reinforced material as claimed in claim 3, it is characterized in that the RF
The preparation method of resin liquid, comprising the following steps:
(1) prepare the formaldehyde 38% of soft water, 22 parts of parts by weight of resorcinol solid and parts by weight 13；
(2) soft water is put into reactor tank, water temperature is controlled at 23 DEG C；
(3) sodium hydroxide is dissolved in soft water, is launched after being configured to the sodium hydrate aqueous solution that concentration is 7% to reactor tank
Interior, sodium hydrate aqueous solution parts by weight are 16 parts, and are stirred 10 minutes；
(4) resorcinol solid is dissolved in soft water, is launched after being configured to the resorcinol solution of concentration 10~20% to anti-
It answers in tank, and is stirred 20 minutes；
(5) formaldehyde 38% is launched into soft water and is mixed, be configured to the formalin that concentration is 5~20%, formaldehyde is water-soluble
Liquid is slowly added in reactor tank, and continues stirred tank；
(6) with 10 DEG C of temperature of the cooling reactor tank of cooling water, control reaction temperature is 20 DEG C, and the reaction time is 12.5 hours, is obtained
To RF resin liquid.
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| 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 |
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