CN102558591B - Preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle - Google Patents
Preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle Download PDFInfo
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Abstract
The invention discloses a preparation method of a fiber-reinforced PCBT (poly cyclic butylene terephthalate) thermoplastic composite material bottom plate for an electric vehicle. According to the method, the reaction time of a ring-opening polymerization reaction of cyclic butylene terephthalate (CBT) resin and a catalyst is improved; the catalyst is loaded on the surface of a fiber fabric instead of being directly added to the CBT resin; and after being heated and melted, the CBT resin is injected into a preheated mould to infiltrate the fiber fabric and simultaneously to be in contact with the catalyst to trigger the ring-opening polymerization reaction. Compared with the prior art, the method has the advantages that a processing time window of fiber-reinforced PCBT composite material products is prolonged, thereby guaranteeing that large thermoplastic fiber-reinforced PCBT composite material products can be prepared under the condition of conventional equipment; and meanwhile, as a matrix of the CBT resin has good infiltration performance, the prepared fiber-reinforced PCBT composite material products have high fiber volume content and excellent mechanical performance, so that the preparation method has great application potential.
Description
Technical field
The present invention relates to fiber-reinforced PC BT technical field of composite materials, relate in particular to a kind of preparation method of large size electro motor-car base plate of fiber-reinforced PC BT matrix material.
Background technology
Along with energy-saving and emission-reduction are rooted in the hearts of the people; people more and more pay attention to effective utilization of environment protection, resource; wherein, adopt superior performance, thermoplastic resin that simultaneously can reshaping replaces traditional thermosetting resin to prepare matrix material as matrix receiving increasing concern.Compared with thermosetting resin, thermoplastic resin has number of important advantages, for example, and recoverable preferably, preferably toughness, shorter shaping cycle and some other noticeable feature.
In-situ polymerization polybutylene terephthalate (PCBT) refers to by annular butylene terephthalate (CBT) resin under suitable temperature and catalyzer condition, carries out the polybutylene terephthalate (PBT) of ring-opening polymerization formation linear macromolecule amount.The fiber-reinforced PC BT thermoplastic composite that continuous fibre and PCBT are compound developed has advantages of that physical strength is higher, weight is lighter, be applicable to being applied to the fields such as trolley part and other products for civilian use, can realize the lightweight of the products such as automobile, thereby effectively save energy, can realize by the method for hot pressing reshaping the recycling of this matrix material, thereby embody the sustainable developability of energy-saving and emission-reduction and the utilization of resources simultaneously.
The method of preparing fiber-reinforced PC BT thermoplastic composite product of generally using is at present by ring-type mutual-phenenyl two acid bromide two alcohol ester (CBT) resin heating and melting, add again catalyzer short mix even, then adopt vacuum assisted resin form (VARI) technique to prepare fiber-reinforced PC BT thermoplastic composite product, first mould is vacuumized, utilize vacuum pressure in the mould of the CBT resin injection preheating of the mixed catalyst of melting, to infiltrate fabric, after completing, resin impregnation process keeps constant temperature, then cooling and demolding, deburring, polishing.But, because CBT resin ring-opening polymerization occurs immediately after contacting with catalyzer, and polymerization rate is very fast, the resin system viscosity of ring-opening polymerization rises rapidly at short notice, after viscosity increases to a certain degree, resin just cannot continue to infiltrate fabric again, therefore utilizes existing method to prepare the process window of fiber-reinforced PC BT thermoplastic composite product very narrow, is only suitable for preparing small size product, be difficult to realize large size product, for example the preparation of power truck base plate.
Summary of the invention
Technical purpose of the present invention be for above-mentioned existing method prepare fiber-reinforced PC BT thermoplastic composite product exist process window narrow, be only suitable for preparing small size product, be difficult to realize the problem of large size product, a kind of preparation method of fiber-reinforced PC BT thermoplastic composite product is provided, the method effectively extends process window, under conventional equipment condition, can realize large size fiber-reinforced PC BT thermoplastic composite product, for example preparation of power truck base plate.
The present invention realizes the technical scheme that above-mentioned technical purpose adopts: a kind of preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle, comprises the following steps:
Step 1: catalyzer is added in solvent and mixed, obtain catalyst solution, adopt the method for spraying by catalyst solution homogeneous immersion fabric, be then dried at 80～100 ℃, solvent is volatilized completely, obtaining area load has the fabric of catalyzer;
Step 2: evenly apply releasing agent after the polishing of power truck base plate die surface, wiped clean, the area load that step 1 is obtained has the fabric of catalyzer to be laid in die surface, and then paving is covered release cloth, flow-guiding screen and airfelt; Then with vacuum bag sealing, cover the above part of whole die surface, sealing region is in communication with the outside by resin inlet tube and resin outlet pipe, resin inlet tube is placed on flow-guiding screen, and resin outlet pipe is placed in airfelt; Clamp resin inlet tube and make whole sealing area airtight, by resin outlet pipe, sealing region is vacuumized to processing;
Step 3: the addition of C BT resin is added in reactor, heat up and make its melting, continue to stir and pass into nitrogen protection, until form the low CBT resin melt of viscosity pole;
Step 4: preheated mold, the CBT resin melt that step 3 is obtained is injected area load by resin inlet tube the fabric of catalyzer, after CBT resin completes impregnation process, constant temperature keeps 15～30min, then cooling and demolding, carry out afterwards deburring, polishing, obtain fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle.
In technique scheme:
Described catalyzer is tin class or titanium class catalyzer, and wherein tin class catalyzer includes but not limited to dihydroxyl dibutyl tin oxide, tin oxygen alkane, in three (2-ethyl-1-caproic acid) butyl tin and 1,1,6, the 6-tetrabutyl-1,6-bis-tin-2,5,7, one or more of 10-tetra-oxygen-cyclodecane, titanium class catalyzer includes but not limited to tetraethyl titanate, titanium propanolate, four (2-Ethylhexyl Alcohol) titanium, one or more of octene di-alcohol titanate and titanium acetylacetone mixture.
As preferably, described catalyst quality accounts for 0.2～1% of CBT resin total mass.
Described solvent includes but not limited to one or more the mixture in trifluoroacetic acid, methylene dichloride, trichloromethane.
The described solvent mixed solvent that preferably trifluoroacetic acid and methylene dichloride are mixed to form as 1: 1～1: 15 take quality proportioning, or the mixed solvent that was mixed to form as 1: 1～1: 15 take quality proportioning of trifluoroacetic acid and trichloromethane.
In described step 2, the vacuum pressure in sealing area preferably remains on 1 standard atmospheric pressure left and right.
In described step 4, die temperature preferably remains on 180～220 ℃.
Continuous-filament woven fabric can be glass fibre and carbon fibre fabric, include but not limited to one or more in plain goods, twilled fabric, satin and sateen cloth, one-way fabric, multi-axial tricot, wherein multi-axial tricot is also referred to as stitch bonded fabric, directly oriented structure fabric or Non crimp fabric.
Compared with the existing method of preparing fiber-reinforced PC BT thermoplastic composite product, the present invention has improved reacting opportunity of CBT resin and catalyzer generation ring-opening polymerization, specific as follows:
In existing technique, first will after CBT resin heating and melting, add catalyzer short mix even, then the mould that injects preheating infiltrates fabric, because CBT resin ring-opening polymerization occurs immediately after contacting with catalyzer, the resin system viscosity that can produce thus ring-opening polymerization rises rapidly at short notice, after viscosity increases to a certain degree, resin just cannot continue to infiltrate fabric again, cause the process window of fiber-reinforced PC BT thermoplastic composite product narrow, the problem that product size is less.
And the research practice of the inventor based on a large amount of sums up, improved reacting opportunity of above-mentioned CBT resin and catalyzer generation ring-opening polymerization,, catalyzer is not directly added in CBT resin, but load on fabric surface, the mould that makes to inject after CBT resin heating and melting preheating contacts with catalyzer ring-opening polymerization occurs when infiltrating fabric, and ring-opening polymerization is synchronizeed and carried out with crystallisation process, and this improvement tool has the following advantages:
(1) can effectively extend CBT resin and infiltrate time of fabric, extend window process period of fiber-reinforced PC BT composite product, thereby guarantee to prepare large size thermoplastic fibre under conventional equipment condition, strengthened PCBT composite product;
(2), because CBT resin matrix has good wetting property, the fiber volume fraction of the fiber-reinforced PC BT composite product preparing is high, has excellent mechanical property.
Accompanying drawing explanation
Fig. 1 is the process structure schematic diagram that embodiment 1 and 2 makes fiber-reinforced PC BT matrix material power truck base plate.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and it is not played to any restriction effect.
Reference numeral in Fig. 1 is: mould 1, releasing agent 2, area load have fabric 3, release cloth 4, flow-guiding screen 5, vacuum bag 6, airfelt 7, sealant tape 8, resin inlet tube 9, resin outlet pipe 10, inlet honeycomb duct 11, the outlet thrust-augmenting nozzle 12 of catalyzer.
Embodiment 1:
In the present embodiment, fiber-reinforced PC BT matrix material large size product is power truck base plate, and mould 1 surface size of this power truck base plate is 160 × 110 square centimeters, is below concrete raw material and preparation process:
The CBT100 resin that CBT resin selects U.S. Cyclics company to produce;
Resin inlet tube 9 all adopts polyfluortetraethylene pipe with resin outlet pipe 10;
Releasing agent 2 adopts
700-NC or AXEL X-807;
Release cloth 4 adopts nylon 66 class materials;
Flow-guiding screen 5, inlet honeycomb duct 11 adopt polyester material with outlet thrust-augmenting nozzle 12;
Vacuum bag 6 adopts nylon 6 class materials;
Airfelt adopts nonwoven polyester class material;
1, cutting fabric: according to power truck base plate mould 1 size cutting glasscloth and carbon fibre fabric successively, quantity, size and the model of fabric are as shown in table 1 below;
Kind, size and the quantity of the fabric using in table 1: embodiment 1
2, Kaolinite Preparation of Catalyst solution: press trifluoroacetic acid: methylene dichloride=1: 10 quality proportioning preparation mixed solvent 500ml, take 25 grams of dihydroxyl dibutyl tin oxides and be dissolved in this mixed solvent, make the catalyst solution of stable homogeneous;
3, prepare area load and have the fabric of catalyzer: the catalyst solution that step 2 is obtained evenly sprays to every one deck fabric surface, then the fabric of processing is put into 80 ℃ of baking ovens dry, mixed solvent is volatilized completely, and obtaining area load has the fabric 3 of catalyzer;
4, mold cleaning and preparation: with 1000 order sand paper by smooth power truck base plate mould 1 surface finish, then with alcohol by die surface wiped clean;
5, coating release agent: the surrounding on mould 1 surface of processing in step 4, paste the sealant tape 8 of appropriate width; On mould 1 surface, the interior even coating releasing agent 2 of sealant tape 8, then standing 20 minutes, repeat this operation 5 times;
6, preparation CBT resin melt: 5000 grams of CBT resins are added in heating container, be warming up to more than 180 ℃, continue mechanical stirring and pass into nitrogen, until its complete melting becomes the CBT resin melt that viscosity pole is low;
7, laid surface load has the fabric of catalyzer: mould 1 surface, the interior paving of sealant tape 8 of processing in step 5 covered area load that step 3 obtains the fabric 3 of catalyzer, laying repeating unit order is followed successively by two-layer T70012K carbon fiber twilled fabric, triplex glass fiber bi-axial fabric, two-layer T70012K carbon fiber twilled fabric from top to bottom, repeats paving and covers five unit;
8, paving is covered auxiliary material: on fabric 3 surfaces of completing, spread successively and cover release cloth 4, flow-guiding screen 5, in sealant tape 8, the both sides of fabric 3 paving is covered airfelt 7, resin inlet tube 9 is placed on flow-guiding screen 5, resin outlet pipe 10 is placed in airfelt 7, has the distance of 2～3cm between airfelt 7 and flow-guiding screen 5;
9, envelope vacuum: cover the surperficial above part of mould 1 with vacuum bag 6, comprise fabric 3, release cloth 4, flow-guiding screen 5, airfelt 7, resin inlet tube 9 and resin outlet pipe 10, vacuum bag 6 peripheries and sealant tape 8 are sealing adhesive, make sealant tape inner compartment sealed air-tight, by resin inlet tube 9 and resin outlet pipe 10, be in communication with the outside, clamping resin inlet tube 9 makes it airtight, outlet thrust-augmenting nozzle 12 by resin outlet pipe 10 vacuumizes sealant tape 8 inner compartments, check the stopping property of package system simultaneously, guarantee without gas leakage, this process is carried out compacting to fiber laying, especially chamfering place,
10, resin infiltrates: utilizing CBT resin melt that vacuum pressure obtains step 6 to inject area load by the inlet honeycomb duct 11 of resin inlet tube 9 has the fabric 3 of catalyzer, whole process die temperature remains on 180 ℃ of left and right, and guarantees that sealing area is air tight;
11, polyreaction: CBT resin melt contacts with catalyzer ring-opening polymerization occurs when infiltrating fabric 3, after CBT resin completes impregnation process, constant temperature keeps getting final product for 15 minutes cooling and demolding, carry out afterwards deburring, polishing, obtain power truck base plate.
The above-mentioned power truck base plate preparing is carried out to following observation and test, obtains corresponding test result:
(1) carry out C-scanning and X-ray check, detected result shows: its internal soundness is even, without bubble and dryspot, exists.
(2) carry out SEM observation, result shows: in microtexture, the associativity of PCBT resin and fortifying fibre is better.In this composite product, fiber volume fraction is approximately 50% left and right.
(3) carry out Elongation test, test result is: tensile strength is approximately 804MPa, and tensile modulus is approximately 68GPa.
(4) carry out three-point bending test, test result is: flexural strength is approximately 500MPa.
(5) carry out interlayer shear test, test result is: interlaminar shear strength is approximately 40MPa.
Embodiment 2:
In the present embodiment, fiber-reinforced PC BT matrix material large size product is power truck base plate, and the die surface 1 of this power truck base plate is of a size of 160 × 110 square centimeters, is below concrete raw material and preparation process:
The CBT100 resin that CBT resin selects U.S. Cyclics company to produce;
Resin inlet tube 9 all adopts polyfluortetraethylene pipe with resin outlet 10 pipes;
Releasing agent 2 adopts
700-NC or AXEL X-807;
Release cloth 4 adopts nylon 66 class materials;
Flow-guiding screen 5, inlet honeycomb duct 11 and outlet thrust-augmenting nozzle 12 adopt polyester material;
Vacuum bag 6 adopts nylon 6 class materials;
1, cutting fabric: according to power truck base plate die size successively cutting glasscloth and carbon fibre fabric, quantity, size and the model of fabric are as shown in table 2 below;
Kind, size and the quantity of the fabric using in table 2: embodiment 2
2, Kaolinite Preparation of Catalyst solution: press trifluoroacetic acid: trichloromethane=1: 8 quality proportioning preparation mixed solvent 500ml, take 40 grams of octene di-alcohol titanates and be dissolved in this mixed solvent, make the catalyst solution of stable homogeneous;
3, prepare area load and have the fabric of catalyzer: the catalyst solution that step 2 is obtained evenly sprays to every one deck fabric surface, then the fabric of processing is put into 80 ℃ of baking ovens dry, mixed solvent is volatilized completely, and obtaining area load has the fabric 3 of catalyzer;
4, mold cleaning and preparation: with 1000 order sand paper by smooth power truck base plate mould 1 surface finish, then with alcohol by die surface wiped clean;
5, coating release agent: the surrounding on mould 1 surface of processing in step 4, paste the sealant tape 8 of appropriate width; On mould 1 surface, the interior even coating releasing agent 2 of sealant tape 8, then standing 20 minutes, repeat this operation 5 times;
6, preparation CBT resin melt: 8000 grams of CBT resins are added in heating container, be warming up to more than 180 ℃, continue mechanical stirring and pass into nitrogen, until its complete melting becomes the CBT resin melt that viscosity pole is low;
7, laid surface load has the fabric of catalyzer: mould 1 surface, the interior paving of sealant tape 8 of processing in step 5 covered area load that step 3 obtains the fabric 3 of catalyzer, laying repeating unit order is followed successively by four layers of T70012K carbon fiber twilled fabric, five layers of glass fibre bi-axial fabric, two-layer T70012K carbon fiber twilled fabric from top to bottom, repeats paving and covers five unit;
8, paving is covered auxiliary material: on fabric 3 surfaces of completing, spread successively and cover release cloth 4, flow-guiding screen 5, in sealant tape 8, the both sides of fabric 3 paving is covered airfelt 7, resin inlet tube 9 is placed on flow-guiding screen 5, resin outlet pipe 10 is placed in airfelt 7, has the distance of 2～3cm between airfelt 7 and flow-guiding screen 5;
9, envelope vacuum: cover the surperficial above part of mould 1 with vacuum bag 6, comprise fabric 3, release cloth 4, flow-guiding screen 5, airfelt 7, resin inlet tube 9 and resin outlet pipe 10, vacuum bag 7 peripheries and sealant tape 8 are sealing adhesive, make sealant tape 8 inner compartment sealed air-tights, by resin inlet tube 9 and resin outlet pipe 10, be in communication with the outside, clamping resin inlet tube 9 makes it airtight, outlet thrust-augmenting nozzle 12 by resin outlet pipe 10 vacuumizes sealant tape 8 inner compartments, check the stopping property of package system simultaneously, guarantee without gas leakage, this process is carried out compacting to fiber laying, especially chamfering place,
10, resin infiltrates: utilizing CBT resin melt that vacuum pressure obtains step 6 to inject area load by the inlet honeycomb duct 11 of resin inlet tube 9 has the fabric 3 of catalyzer, whole process mould 1 temperature remains on 180 ℃ of left and right, and guarantees that sealing area is air tight;
11, polyreaction: CBT resin melt contacts with catalyzer ring-opening polymerization occurs when infiltrating fabric 3, after CBT resin completes impregnation process, constant temperature keeps 15min to get final product cooling and demolding, carries out afterwards deburring, polishing, obtains power truck base plate.
The above-mentioned power truck base plate preparing is carried out to following observation and test, obtains corresponding test result:
(1) carry out C-scanning and X-ray check, detected result shows: its internal soundness is even, without bubble and dryspot, exists.
(2) carry out SEM observation, result shows: in microtexture, the associativity of PCBT resin and fortifying fibre is better.In this composite product, fiber volume fraction is approximately 50% left and right.
(3) carry out Elongation test, test result is: tensile strength is approximately 950MPa, and tensile modulus is approximately 80GPa.
(4) carry out three-point bending test, test result is: flexural strength is approximately 600MPa.
(5) carry out interlayer shear test, test result is: interlaminar shear strength is approximately 45MPa.
Above-described embodiment has been described in detail technical scheme of the present invention and beneficial effect; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any modifications of making within the scope of principle of the present invention and improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. a preparation method for fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle, is characterized in that: comprise the following steps:
Step 1: catalyzer is added in solvent and mixed, obtain catalyst solution, adopt the method for spraying by catalyst solution homogeneous immersion fabric, be then dried at 80～100 ℃, solvent is volatilized completely, obtaining area load has the fabric of catalyzer;
Described catalyzer is tin class or titanium class catalyzer, and wherein tin class catalyzer comprises dihydroxyl dibutyl tin oxide, tin oxygen alkane, three (2-ethyl-1-caproic acid) butyl tin and 1,1,6, the 6-tetrabutyl-1,6-bis-tin-2, one or more of 5,7,10-, tetra-oxygen-cyclodecane; Titanium class catalyzer comprises tetraethyl titanate, titanium propanolate, four (2-Ethylhexyl Alcohol) titanium, one or more of octene di-alcohol titanate and titanium acetylacetone mixture;
Described solvent comprises one or more the mixture in trifluoroacetic acid, methylene dichloride, trichloromethane;
Step 2: evenly apply releasing agent after the polishing of power truck base plate die surface, wiped clean, the area load that step 1 is obtained has the fabric of catalyzer to be laid in die surface, and then paving is covered release cloth, flow-guiding screen and airfelt; Then with vacuum bag sealing, cover the above part of whole die surface, sealing area is in communication with the outside by resin inlet tube and resin outlet pipe, resin inlet tube is placed on flow-guiding screen, and resin outlet pipe is placed in airfelt; Clamp resin inlet tube and make whole sealing area airtight, by resin outlet pipe, sealing area is vacuumized to processing;
Step 3: the addition of C BT resin is added in reactor, heat up and make its melting, continue to stir and pass into nitrogen protection, until form the low CBT resin melt of viscosity pole;
Step 4: preheated mold, the CBT resin melt that step 3 is obtained is injected area load by resin inlet tube the fabric of catalyzer, after CBT resin impregnation process completes, constant temperature keeps 15～30min, then cooling and demolding, carry out afterwards deburring, polishing, obtain fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle; Described catalyst quality accounts for 0.2～1% of CBT resin total mass.
2. the preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle according to claim 1, is characterized in that: described fabric comprises glass fibre and carbon fibre fabric.
3. the preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle according to claim 1, is characterized in that: described fabric comprises one or more in plain goods, twilled fabric, satin and sateen cloth, one-way fabric, multi-axial tricot.
4. the preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle according to claim 1, is characterized in that: in described step 2, the vacuum pressure in sealing area remains on 1 standard atmospheric pressure.
5. the preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle according to claim 1, is characterized in that: in described step 4, die temperature remains on 180～220 ℃.
6. the preparation method of fiber-reinforced PCBT thermoplastic composite material bottom plate for electric vehicle according to claim 1, it is characterized in that: described solvent is the mixed solvent that trifluoroacetic acid and methylene dichloride are mixed to form take quality proportioning as 1:1～1:15, or the mixed solvent that is mixed to form take quality proportioning as 1:1～1:15 of trifluoroacetic acid and trichloromethane.
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| CN104098875B (en) * | 2013-04-09 | 2017-10-17 | 上海杰事杰新材料(集团)股份有限公司 | A kind of continuous lod CBT prepreg tapes and its preparation method and application |
| CN104262593B (en) * | 2014-03-14 | 2016-08-31 | 深圳航天科技创新研究院 | A kind of cyclic oligomer composite material and in-situ preparation method thereof |
| CN104130393A (en) * | 2014-07-04 | 2014-11-05 | 中国科学院宁波材料技术与工程研究所 | Continuous fiber enhanced thermoplastic composite material prepreg tape preparation method and device for realizing the method |
| JP6942000B2 (en) * | 2017-08-01 | 2021-09-29 | 株式会社日立製作所 | Fiber reinforced plastic and its manufacturing method |
| CN113085221B (en) * | 2021-03-29 | 2022-04-26 | 北京化工大学 | Continuous fiber reinforced thermoplastic resin vacuum bag pressing forming device and method |
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| CN102166825A (en) * | 2010-12-24 | 2011-08-31 | 中国科学院宁波材料技术与工程研究所 | Technology of making automobile engine cover with carbon fiber reinforcement resin-based composite material |
| CN102166826A (en) * | 2011-01-19 | 2011-08-31 | 中国科学院宁波材料技术与工程研究所 | Forming process of fiber reinforced thermoplastic composite material |
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| CN102166825A (en) * | 2010-12-24 | 2011-08-31 | 中国科学院宁波材料技术与工程研究所 | Technology of making automobile engine cover with carbon fiber reinforcement resin-based composite material |
| CN102166826A (en) * | 2011-01-19 | 2011-08-31 | 中国科学院宁波材料技术与工程研究所 | Forming process of fiber reinforced thermoplastic composite material |
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