CN104098875B - A kind of continuous lod CBT prepreg tapes and its preparation method and application - Google Patents
A kind of continuous lod CBT prepreg tapes and its preparation method and application Download PDFInfo
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- CN104098875B CN104098875B CN201310120647.3A CN201310120647A CN104098875B CN 104098875 B CN104098875 B CN 104098875B CN 201310120647 A CN201310120647 A CN 201310120647A CN 104098875 B CN104098875 B CN 104098875B
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Abstract
The invention belongs to technical field of polymer composite materials, it is related to a kind of continuous lod CBT prepreg tapes and its preparation method and application.Continuous lod CBT prepreg tapes are made up of the component comprising following parts by weight：100~235 parts of 100 parts of CBT resins, 0~0.6 part of catalyst and continuous fiber.The relatively low catalyst of activity is selected in the present invention, CBT resins and catalyst is set not to react in an extruder or difficult reaction, resin extruded melt impregnation method is recycled to prepare continuous lod CBT prepreg tapes, the power consumption of this technology is low, environmental pollution is few, and the preimpregnation tape thickness of preparation is uniform, and fiber content is high, the good prepreg tape of resin effect of impregnation, and physical property preferably composite is prepared by staircase response.
Description
Technical field
The invention belongs to technical field of polymer composite materials, it is related to a kind of continuous lod CBT prepreg tapes and its system
Preparation Method and application.
Background technology
CBT resins, i.e. cyclic butylene terephthalate, CBT are Cyclic butylenes terephthalate
Abbreviation.CBT resins, oligomer is generally 2~5 aggressiveness, due to its unique loop configuration feature, and its processing viscosity is very low,
It can reach that intimate small molecule liquid water is the same, this is easy to the dipping of fiber and filler, be conducive to producing long-range thin-walled system
Product.According to catalyst and the difference of reaction temperature, the complete reaction time can be controlled in tens seconds in dozens of minutes, and can basis
The demand of application selects different catalyst type and reaction temperature；There is no the release of chemical substance in course of reaction, be one
Environment-friendly material is planted, while also easily obtaining bright and clean surface；There is no the generation of reaction heat in course of reaction, it is easy to the control of reaction
System, can prepare large scale product, shorten molding cycle；It is easy to hot forming simultaneously, forming process is simplified, when shortening processing
Between；PBT, the plastics obtained after polymerization have preferable rigidity, toughness, heat-resisting, resistant to chemical etching, dimensional stability, electricity absolutely
Edge is good, fire-retardant, thermoformable, convenient and recycling post-processing the advantages of.
General work in-process thermoplastic matrix primary disadvantage is that its high viscosity, this has had a strong impact on fibre reinforcement
Dipping, CBT resins can just solve highly viscous problem during pre-soaking fiber.It is compound that continuous lod CBT is obtained
The characteristics of material combines thermoplastic and thermosetting resin, therefore have broad application prospects.Such as using CBT resins as base
The fibrous composite of body manufacture can make the blade of wind-driven generator, and its blade has that impact resistance is high, shaping speed is fast, valency
The advantages of lattice are economic.
At present, the conventional method for preparing continuous lod CBT composites has vacuum assisted resin form
（VARI）, solvent method and resin film method etc., vacuum assisted resin form is by the CBT resins of melting using vacuum pressure
With wetting fibre or fabric in catalyst injection mould, the method is only suitable for the preparation of small size product, is difficult to realize big
The preparation of size product；Solvent method is all to dissolve CBT resins and catalyst in a solvent, then allows fiber or fabric to exist
Impregnated in solution, or by solution spraying on fiber or fabric, then through drying, solvent is volatilized completely, but volatilization
Solvent can cause environmental pollution；And resin film method is that CBT resins first are prepared into film using blowing or the tape casting, then by its
With fiber or fabric hot melt it is laminating prepare composite, film-forming process adds the input of equipment, also increases energy consumption.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of continuous lod
CBT prepreg tapes and its preparation method and application.
The present invention combines existing continuous fiber reinforced thermoplastic resin composite material presoaked belt production equipment, the active phase of selection
To relatively low catalyst, using resin extruded fusion method impregnating continuous fibres, so as to prepare, thickness is uniform, and fiber content is higher,
The prepreg tape and its composite of better performances.
To achieve the above object, the present invention uses following technical scheme：
A kind of continuous lod cyclic butylene terephthalate（CBT）Prepreg tape, by including following parts by weight
Component is made：
100 parts of cyclic butylene terephthalate,
0~0.6 part of catalyst,
100~235 parts of continuous fiber.
The content of the catalyst is 0.2~0.6 part.
Described cyclic butylene terephthalate is cyclic butylene terephthalate, preferably the model U.S.
CBT100, CBT160 or CBT200 of Cyclics companies production, wherein CBT100 and CBT200 are free of catalyst, and CBT160 contains
There is the tin catalyst of 0.25% molar concentration.
Described catalyst is titanium class catalyst or tin catalyst, preferably four（2- ethyl -1,3- hexylene glycols）Close titanium, two
（Levulinic ketone group）It is metatitanic acid diisopropyl ester, double（Ethyl acetoacetate）Metatitanic acid diisopropyl ester, dihydroxy dibutyl tin oxide or only son
The isooctyl acid tin of base three.
Described continuous fiber is selected from glass fibre, carbon fiber, boron fibre or basalt fibre.
A kind of preparation method of above-mentioned continuous lod cyclic butylene terephthalate prepreg tape, including following step
Suddenly：
（1）100 parts of dry cyclic butylene terephthalates and 0~0.6 part of catalyst are well mixed；
（2）By step（1）The extruded machine extrusion of middle compound, and allow the melting cyclic butylene terephthalate of extrusion
Resin meets with 100~235 parts of continuous fibers at double extrusion dies that extruder interlocks, and dipping is realized, then by prepreg tape
Drawn by cold pressing roller, wind, obtain impregnating complete continuous lod cyclic butylene terephthalate prepreg tape.
Described step（1）The drying condition of middle cyclic butylene terephthalate is：Dried in 80~100 DEG C of baking ovens
8~12h；
Described step（1）The device of middle mixing is high-speed mixer, and incorporation time is 3~7min；
Described step（2）In the extruder used be continuous fiber reinforced thermoplastic resin composite material presoaked belt system
Standby equipment（Equipment disclosed in patent CN101474868A）, extruder screw rotating speed is 10~150r/min, melting extrusion temperature
Spend for 150~190 DEG C, hauling speed is 2~10m/min.
One kind utilizes composite made from above-mentioned continuous lod cyclic butylene terephthalate prepreg tape.
A kind of preparation method of above-mentioned composite, comprises the following steps：
Above-mentioned continuous lod cyclic butylene terephthalate prepreg tape is needed to be cut according to reality, spread
Layer, it is hot-forming on vulcanizing press, composite is taken out after cold pressing, and survey its physical property.
Described hot-forming condition is：200~240 DEG C of temperature, pressure is 0~5MPa, and the time is 30~90min；
The pressure of described cold pressing is 5MPa, and the time is 30~60min.
Device used in this application is the Preparation equipment of continuous fiber reinforced thermoplastic resin composite material presoaked belt（Its is special
Sharp Publication No. CN101474868A）In this application, continuous lod CBT prepreg tapes are prepared using this equipment, not only consumed
Can be relatively low, environmental pollution is few, but also can control prepreg tape according to extruder screw rotating speed and hauling machine hauling speed
Gel content, the prepreg tape thickness error of preparation can be controlled in ± 0.02mm, and fiber content can be up to more than 70%, production effect
Rate is also higher.By fiber reinforcement CBT preimpregnation materials lamination as needed, molding, composite finished product is made in thermal polymerization, so that
The application field of CBT resins is expanded.
Compared with prior art, the present invention has advantages below and beneficial effect：
（1）In the present invention, continuous lod CBT prepreg tapes are prepared using resin extruded melt impregnation method, not only consumed
Can be relatively low, environmental pollution is few, but also can control prepreg tape according to extruder screw rotating speed and hauling machine hauling speed
Gel content, the prepreg tape thickness error of preparation can be controlled in ± 0.02mm, and fiber content can be up to more than 70%, production effect
Rate is also higher.
（2）The relatively low catalyst of activity is selected in the present invention, CBT resins and catalyst is tried one's best in an extruder not
Reaction or difficult reaction, prepare the good prepreg tape of resin effect of impregnation, and be preferably combined by staircase response preparation physical property
Material.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
In following examples, the tensile property of products obtained therefrom is tested according to standard ASTM D3039, and bending property is according to mark
Quasi- ASTM D7264 tests, interlaminar shear strength is tested according to standard ASTM D2344.
Embodiment 1
（1）CBT160 is first dried into 12h in 80 DEG C of baking ovens, then take dried 100 parts of CBT160 resins (plus
The tin catalyst of 0.25% molar concentration）；
（2）By step（1）The middle extruded machine of CBT160 resins（Patent CN101474868A is designed）Extrusion, and allow extrusion
Melting CBT160 resins meet with 100 parts of basalt fibres at double extrusion dies staggeredly, dipping are realized, then by prepreg tape
Draw, wind, you can obtain impregnating complete continuous lod CBT resin prepreg bands, wherein extruder spiral shell by cold pressing roller
Bar rotating speed is 10r/min, and melting extrusion temperature is：One 150 DEG C of area, two 165 DEG C of areas, three 170 DEG C of areas, four 180 DEG C of areas, 5th area
190 DEG C, 190 DEG C of head, hauling speed is 2m/min；
（3）Above-mentioned prepreg tape is needed to be cut according to reality, laying, hot-forming on vulcanizing press, cold pressing
After take out composite, and survey its physical property（It is shown in Table 1）, wherein hot-forming condition：Kept under 220 DEG C of no pressures of temperature
20min, then keeps 10min under 240 DEG C, 5MPa, is cold-pressed condition：Pressure is 5MPa, and the time is 30min.
Embodiment 2
（1）CBT100 is first dried into 10h in 90 DEG C of baking ovens, then takes dried 100 parts of CBT100 resins and 0.2 part
Catalyst four（2- ethyl -1,3- hexylene glycols）Close titanium and 3min is mixed in high-speed mixer, be well mixed；
（2）By step（1）The middle extruded machine of compound（Patent CN101474868A is designed）Extrusion, and allow the melting of extrusion
CBT100 resins meet with 150 parts of boron fibres at double extrusion dies staggeredly, realize dipping, then by prepreg tape by being cold-pressed
Roller is drawn, winding, you can obtain impregnating complete continuous lod CBT100 resin prepreg bands, wherein extruder screw rotating speed
For 45r/min, melting extrusion temperature is：One 150 DEG C of area, two 165 DEG C of areas, three 170 DEG C of areas, four 180 DEG C of areas, five 190 DEG C of areas, machine
First 190 DEG C, hauling speed is 4m/min；
（3）Above-mentioned prepreg tape is needed to be cut according to reality, laying, hot-forming on vulcanizing press, cold pressing
After take out composite, and survey its physical property（It is shown in Table 1）, keep 30min under 220 DEG C of no pressures of temperature, then 240 DEG C,
20min is kept under 4MPa, condition is cold-pressed：Pressure is 5MPa, and the time is 40min.
Embodiment 3
（1）CBT200 is first dried into 8h in 100 DEG C of baking ovens, then takes dried 100 parts of CBT200 resins and 0.3 part
Catalyst two（Levulinic ketone group）Metatitanic acid diisopropyl ester mixes 4min in high-speed mixer, is well mixed；
（2）By step（1）The middle extruded machine of compound（Patent CN101474868A is designed）Extrusion, and allow the melting of extrusion
CBT200 resins meet with 167.5 parts of glass fibres at double extrusion dies staggeredly, realize dipping, then pass through prepreg tape
Cold pressing roller is drawn, winding, you can obtain impregnating complete continuous lod CBT200 resin prepreg bands, wherein extruder screw
Rotating speed is 80r/min, and melting extrusion temperature is：One 150 DEG C of area, two 165 DEG C of areas, three 170 DEG C of areas, four 180 DEG C of areas, five areas 185
DEG C, 185 DEG C of head, hauling speed is 6m/min；
（3）Above-mentioned prepreg tape is needed to be cut according to reality, laying, hot-forming on vulcanizing press, cold pressing
After take out composite, and survey its physical property（It is shown in Table 1）, keep 40min under 200 DEG C of no pressures of temperature, then 220 DEG C,
20min is kept under 2.5MPa, then 10min is kept under 230 DEG C, 5MPa, condition is cold-pressed：Pressure is 5MPa, and the time is 45min.
Embodiment 4
（1）CBT100 is first dried into 12h in 80 DEG C of baking ovens, then takes dried 100 parts of CBT100 resins and 0.4 part
Catalyst is double（Ethyl acetoacetate）Metatitanic acid diisopropyl ester mixes 5min in high-speed mixer, is well mixed；
（2）By step（1）The middle extruded machine of compound（Patent CN101474868A is designed）Extrusion, and allow the melting of extrusion
CBT100 resins meet with 235 parts of carbon fibers at double extrusion dies staggeredly, realize dipping, then by prepreg tape by being cold-pressed
Roller is drawn, winding, you can obtain impregnating complete continuous lod CBT100 resin prepreg bands, wherein extruder screw rotating speed
For 115r/min, melting extrusion temperature is：One 150 DEG C of area, two 165 DEG C of areas, three 170 DEG C of areas, four 180 DEG C of areas, five 190 DEG C of areas,
190 DEG C of head, hauling speed is 8m/min；
（3）Above-mentioned prepreg tape is needed to be cut according to reality, laying, hot-forming on vulcanizing press, cold pressing
After take out composite, and survey its physical property（It is shown in Table 1）, keep 40min under 200 DEG C of no pressures of temperature, then 220 DEG C,
30min is kept under 2.5MPa, then 10min is kept under 240 DEG C, 5MPa, condition is cold-pressed：Pressure is 5MPa, and the time is 50min.
Embodiment 5
（1）CBT100 is first dried into 10h in 90 DEG C of baking ovens, then takes dried 100 parts of CBT100 resins and 0.6 part
Catalyst dihydroxy dibutyl tin oxide mixes 6min in high-speed mixer, is well mixed；
（2）By step（1）The middle extruded machine of compound（Patent CN101474868A is designed）Extrusion, and allow the melting of extrusion
CBT100 resins meet with 185 parts of glass fibres at double extrusion dies staggeredly, realize dipping, then by prepreg tape through supercooling
Pressure roller is drawn, winding, you can obtain impregnating complete continuous lod CBT100 resin prepreg bands, wherein extruder screw turns
Speed is 150r/min, and melting extrusion temperature is：One 150 DEG C of area, two 165 DEG C of areas, three 170 DEG C of areas, four 180 DEG C of areas, five areas 190
DEG C, 190 DEG C of head, hauling speed is 10m/min；
（3）Above-mentioned prepreg tape is needed to be cut according to reality, laying, hot-forming on vulcanizing press, cold pressing
After take out composite, and survey its physical property（It is shown in Table 1）, keep 50min under 200 DEG C of no pressures of temperature, then 220 DEG C,
30min is kept under 2.5MPa, then 10min is kept under 240 DEG C, 5MPa, condition is cold-pressed：Pressure is 5MPa, and the time is 60min.
Embodiment 6
（1）CBT100 is first dried into 8h in 100 DEG C of baking ovens, then takes dried 100 parts of CBT100 resins and 0.6 part
The isooctyl acid tin of catalyst monobutyl three mixes 7min in high-speed mixer, is well mixed；
（2）By step（1）The middle extruded machine of compound（Patent CN101474868A is designed）Extrusion, and allow the melting of extrusion
CBT100 resins meet with 235 parts of glass fibres at double extrusion dies staggeredly, realize dipping, then by prepreg tape through supercooling
Pressure roller is drawn, winding, you can obtain impregnating complete continuous lod CBT100 resin prepreg bands, wherein extruder screw turns
Speed is 115r/min, and melting extrusion temperature is：One 150 DEG C of area, two 165 DEG C of areas, three 170 DEG C of areas, four 180 DEG C of areas, five areas 190
DEG C, 190 DEG C of head, hauling speed is 8m/min；
（3）Above-mentioned prepreg tape is needed to be cut according to reality, laying, hot-forming on vulcanizing press, cold pressing
After take out composite, and survey its physical property（It is shown in Table 1）, keep 50min under 200 DEG C of no pressures of temperature, then 220 DEG C,
30min is kept under 2.5MPa, then 10min is kept under 240 DEG C, 5MPa, condition is cold-pressed：Pressure is 5MPa, and the time is 60min.
Embodiment 7
（1）CBT100 is first dried into 8h in 100 DEG C of baking ovens, then takes dried 100 parts of CBT100 resins and 0.2 part
The isooctyl acid tin of catalyst monobutyl three mixes 7min in high-speed mixer, is well mixed；
（2）By step（1）The middle extruded machine of compound（Patent CN101474868A is designed）Extrusion, and allow the melting of extrusion
CBT100 resins meet with 235 parts of glass fibres at double extrusion dies staggeredly, realize dipping, then by prepreg tape through supercooling
Pressure roller is drawn, winding, you can obtain impregnating complete continuous lod CBT100 resin prepreg bands, wherein extruder screw turns
Speed is 115r/min, and melting extrusion temperature is：One 150 DEG C of area, two 165 DEG C of areas, three 170 DEG C of areas, four 180 DEG C of areas, five areas 190
DEG C, 190 DEG C of head, hauling speed is 8m/min；
（3）Above-mentioned prepreg tape is needed to be cut according to reality, laying, hot-forming on vulcanizing press, cold pressing
After take out composite, and survey its physical property（It is shown in Table 1）, keep 50min under 200 DEG C of no pressures of temperature, then 220 DEG C,
30min is kept under 2.5MPa, then 10min is kept under 240 DEG C, 5MPa, condition is cold-pressed：Pressure is 5MPa, and the time is 60min.
The performance of the continuous lod CBT composites of table 1
The embodiment 1~4 from table 1 is as can be seen that physical property and the fiber reinforcement of continuous lod CBT composites
Body is relevant；From embodiment 5,6 as can be seen that composite physical property it is relevant with fibre reinforcement content, fiber content compared with
Gao Shi, tensile strength, bending strength and bending modulus are also higher, but interlaminar shear strength is relatively low, because interlayer shear is strong
Fiber is relevant with the adhesion strength of interlaminar resin with resin, resin in degree and composite interlayer, and resin content reduction is too many, bonds
Intensity also decreases；From embodiment 6,7 as can be seen that when catalyst content is relatively low, can also influence the physical of composite
Energy.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using this hair
It is bright.Person skilled in the art obviously can make various modifications easily to these embodiments, and described herein
General Principle is applied in other embodiment without passing through performing creative labour.Therefore, the invention is not restricted to implementation here
Example, those skilled in the art do not depart from improvement that scope made and change all should be according to the announcement of the present invention
Within protection scope of the present invention.
Claims (6)
1. a kind of continuous lod cyclic butylene terephthalate prepreg tape, it is characterised in that：Include following parts by weight
Component：
100 parts of cyclic butylene terephthalate,
0.2~0.6 part of catalyst,
100~235 parts of continuous fiber；
Described catalyst is titanium class catalyst or tin catalyst；
The titanium class catalyst be selected from four (2- ethyl -1,3- hexylene glycols) close titanium, two (levulinic ketone group) metatitanic acid diisopropyl esters or
Double (ethyl acetoacetate) metatitanic acid diisopropyl esters；
The tin catalyst is dihydroxy dibutyl tin oxide；
Described continuous fiber is selected from carbon fiber, boron fibre or basalt fibre；
The preparation method of described continuous lod cyclic butylene terephthalate prepreg tape comprises the following steps：
(1) 100 parts of dry cyclic butylene terephthalates and 0.2~0.6 part of catalyst are well mixed；
(2) the extruded machine of compound in step (1) is extruded, and allows the melting cyclic butylene terephthalate resin of extrusion
Met with 100~235 parts of continuous fibers at double extrusion dies that extruder interlocks, realize dipping, then pass through prepreg tape
Cold pressing roller is drawn, winding, obtains impregnating complete continuous lod cyclic butylene terephthalate prepreg tape；
The drying condition of cyclic butylene terephthalate is in described step (1)：Dry 8 in 80~100 DEG C of baking ovens~
12h；
The extruder used in described step (2) sets for the preparation of continuous fiber reinforced thermoplastic resin composite material presoaked belt
Standby, extruder screw rotating speed is 10~150r/min, and melting extrusion temperature is 150~190 DEG C, and hauling speed is 2~10m/
min。
2. continuous lod cyclic butylene terephthalate prepreg tape according to claim 1, it is characterised in that：
Model CBT100, CBT160 or CBT200 of described cyclic butylene terephthalate.
3. a kind of preparation side of the continuous lod cyclic butylene terephthalate prepreg tape described in claim 1 or 2
Method, it is characterised in that：Comprise the following steps：
(1) 100 parts of dry cyclic butylene terephthalates and 0.2~0.6 part of catalyst are well mixed；
(2) the extruded machine of compound in step (1) is extruded, and allows the melting cyclic butylene terephthalate resin of extrusion
Met with 100~235 parts of continuous fibers at double extrusion dies that extruder interlocks, realize dipping, then pass through prepreg tape
Cold pressing roller is drawn, winding, obtains impregnating complete continuous lod cyclic butylene terephthalate prepreg tape；
The drying condition of cyclic butylene terephthalate is in described step (1)：Dry 8 in 80~100 DEG C of baking ovens~
12h；
The extruder used in described step (2) sets for the preparation of continuous fiber reinforced thermoplastic resin composite material presoaked belt
Standby, extruder screw rotating speed is 10~150r/min, and melting extrusion temperature is 150~190 DEG C, and hauling speed is 2~10m/
min。
4. preparation method according to claim 3, it is characterised in that：The device of mixing is at a high speed in described step (1)
Mixer, incorporation time is 3~7min.
5. the continuous lod cyclic butylene terephthalate prepreg tape described in a kind of utilization claim 1 or 2 is made
Composite.
6. a kind of preparation method of the composite described in claim 5, it is characterised in that：Comprise the following steps：
By continuous lod cyclic butylene terephthalate prepreg tape cutting, laying, the heat on vulcanizing press
It is molded, cold pressing；Wherein described hot-forming condition is：200~240 DEG C of temperature, pressure be 0~5MPa, the time be 30~
90min；The pressure of described cold pressing is 5MPa, and the time is 30~60min.
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| CN201310120647.3A CN104098875B (en) | 2013-04-09 | 2013-04-09 | A kind of continuous lod CBT prepreg tapes and its preparation method and application |
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| CN107345602B (en) * | 2016-05-04 | 2020-10-16 | 广州金发碳纤维新材料发展有限公司 | Flexible composite pipe and manufacturing method thereof |
| CN109971138B (en) * | 2019-03-22 | 2021-08-17 | 江门市德山复合材料科技有限公司 | Self-repairing PCBT composite material and preparation method thereof |
| CN112480611B (en) * | 2020-11-27 | 2023-03-21 | 金发科技股份有限公司 | Low-emission long glass fiber reinforced PCBT material and preparation method thereof |
| CN114561099B (en) * | 2022-04-19 | 2024-03-08 | 宁海宏德新材料科技有限公司 | Solar cell frame material and preparation method thereof |
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| CN102555234A (en) * | 2012-02-01 | 2012-07-11 | 中材科技风电叶片股份有限公司 | Resin membrane melt impregnation forming method of fiber reinforced PBT composite material |
| CN102558591A (en) * | 2011-12-22 | 2012-07-11 | 中国科学院宁波材料技术与工程研究所 | Preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle |
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| US20050095415A1 (en) * | 2003-10-30 | 2005-05-05 | Raghavendran Venkat K. | Glass mat thermoplastic composite |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558591A (en) * | 2011-12-22 | 2012-07-11 | 中国科学院宁波材料技术与工程研究所 | Preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle |
| CN102555234A (en) * | 2012-02-01 | 2012-07-11 | 中材科技风电叶片股份有限公司 | Resin membrane melt impregnation forming method of fiber reinforced PBT composite material |
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Denomination of invention: Continuous fiber-enhanced CBT prepreg, and preparation method and application thereof Effective date of registration: 20191202 Granted publication date: 20171017 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980000815 |
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