CN102558701A - Method for preparing transparent thermoplastic glass fiber reinforced plastic sheet - Google Patents
Method for preparing transparent thermoplastic glass fiber reinforced plastic sheet Download PDFInfo
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- CN102558701A CN102558701A CN2010105806393A CN201010580639A CN102558701A CN 102558701 A CN102558701 A CN 102558701A CN 2010105806393 A CN2010105806393 A CN 2010105806393A CN 201010580639 A CN201010580639 A CN 201010580639A CN 102558701 A CN102558701 A CN 102558701A
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Abstract
The invention relates to a method for preparing a highly-transparent thermoplastic glass fiber reinforced plastic sheet. The method comprises the following steps: 1, preparing a prepolymerization solution; 2, dipping glass fibers in the prepolymerization solution, and carrying out die locking; 2, carrying out compression molding by arranging a molding die on a press until complete solidification; and 3, polishing burrs, and straightening the circumferences to obtain the transparent thermoplastic glass fiber reinforced plastic sheet. According to the invention, the refractive index of a polymer matrix is adjusted through adjusting the ratio of methyl methacrylate to styrene, so the refractive index of the matrix is highly consistent with the refractive index of the glass fibers, thereby the highly-transparent thermoplastic glass fiber reinforced plastic sheet is prepared. The viscosity of above dipping solution can be freely controlled through adopting a prepolymerization process, so the viscosity of the dipping solution can be freely controlled, the dipping effect to the glass fiber is very good, the glass fibers in the molded transparent glass fiber reinforced plastic cannot be visually observed, and the highest light transmittance can reach 90%. No crosslinking reaction is carried out in the solidification process, and the obtained thermoplastic glass fiber reinforced plastic sheet has a precious secondary thermal deformation characteristic.
Description
Technical field
The invention belongs to the FRP technology field, relate to a kind of preparation method of reinforced plastic plate.
Background technology
The transparent glass steel is a kind of galss fiber reinforced resin based composites, not only has HS, the high-modulus characteristics of glass reinforced plastic, and has good light transmittance, can be used as the construction that lighting material is used for transparent square, transparent worker-house, transparent green house of vegetables.Usually, transparent grp is to adopt the compound and preparation of thermosetting resin and spun glass, shortcoming be glass reinforced plastic in case typing can not change shape through heating again, do not possess the ability of secondary temperature distortion, and be difficult to recycling.In addition, because the inherent defect of thermosetting resin, the shock resistance of thermoset transparent glass steel is relatively poor.Chinese patent 00121534.5 discloses a kind of making method of transparent glass fiber reinforced plastic board for basketball stand; Chinese patent 200710044467.6 discloses a kind of preparation method of light transparent and flame retardant changeable glass reinforced plastic; Chinese patent 02132502.2 discloses the full impregnated formed material that is used for non-alkali cloth reinforced plastics; In addition, Chinese patent 200610086258.3 has been described a kind of transparent glass fibre reinforced plastic grille and working method thereof.None is not to adopt the matrix of thermosetting resin as glass reinforced plastic for above-mentioned patent.Although Chinese patent 200510041290.5 has been told about a kind of pultrusion method and shaping mould thereof of thermoplastic composite.But the method that this patent adopts is to utilize the union yarn of organic fibre and spun glass to carry out pultrusion, produces continuous section bar.Because the melt viscosity of polymkeric substance is very big, a significant disadvantage of this method is in the pultrusion process, and the fused organic fibre is difficult to the spun glass thorough impregnation, and this can have influence on the light transmission of product.
Summary of the invention
The objective of the invention is to the defective of prior art and a kind of printing opacity fiber glass reinforced thermoplastics preparation of plates method is provided.
The present invention adopts following technical scheme:
Key problem in technology of the present invention is that requirement resin matrix and glass specific refractory power are wanted matched, and the error of specific refractory power that makes resin matrix and glass is less than 0.1%.
The specific refractory power of copolymer resins can roughly be estimated according to following formula:
Specific refractory power=the n of multipolymer
(PMMA)* W%
(PMMA)+ n
(PS)* W%
(PS)
In the above formula:
n
(PMMA)Be the specific refractory power of pure polymethylmethacrylate (PMMA), this value gets 1.490;
W%
(PMMA)Weight ratio for PMMA in the multipolymer;
n
(PS)Be the specific refractory power of pure PS (PS), this value gets 1.591.
W%
(PS)Weight ratio for PS in the multipolymer;
The monomer ratio of utilizing above formula to calculate can only roughly be confirmed a scope; Also to consider the influence of modified monomer, releasing agent and softening agent to the resin specific refractory power; Because of the specific refractory power of releasing agent, softening agent and modified monomer lower; Add these auxiliary agents and can reduce the specific refractory power of resin matrix to a certain extent, so in actual prescription, should suitably strengthen cinnamic consumption.
Concrete grammar is: at first through calculating rough confirm TEB 3K and cinnamic proportioning; Add the consumption of modified monomer, initiator, releasing agent, softening agent and fixing these auxiliary agents then, carry out radical polymerization, after question response is complete; Utilize Abbe refractometer to measure the specific refractory power of resulting polymers; If the gained specific refractory power is lower than the specific refractory power of glass, then suitably increase cinnamic consumption, be higher than the specific refractory power of glass like the gained specific refractory power; Then suitably reduce cinnamic consumption, be lower than 0.1% until the specific refractory power of resinous substrates and the specific refractory power error of glass.
A kind of method of manufacture of high printing opacity fiber glass reinforced thermoplastics sheet material comprises step:
(1) preparation of pre-polymerization liquid:
TEB 3K, vinylbenzene and modified monomer are mixed according to the certainweight ratio, add releasing agent, softening agent, initiator, start and stir, in polymeric kettle, carry out radical polymerization, treat that viscosity obviously begins to rise after, reduce to room temperature, pre-polymerization liquid;
(2) impregnated glass fiber:
Glass fiber material successively is laid in the mould, successively floods with pre-polymerization liquid, then matched moulds;
(3) molded curing:
At a certain temperature, forming mould is placed on carries out compression molding on the press, until completely solidified;
(4) polishing burr, periphery is repaiied directly:
After the completely solidified, take out reinforced plastic plate, utilize emery wheel that burr are polished smooth, can obtain the translucent glass fibre board material.
The temperature of described polymerization reaction kettle is 50～90 ℃.
The described pre-polymerization time is 1～16 hour.
Described mould temperature control is at 60～120 ℃.
The viscosity of described pre-polymerization liquid is no more than 0.1Pa.S.
Described TEB 3K and cinnamic weight ratio are decided by the specific refractory power of used glass, make the error of specific refractory power of specific refractory power and the glass of formed polymkeric substance after the complete polymerization of pre-polymerization liquid be no more than 0.1%.
Described modified monomer is SY-Monomer G or maleic anhydride, and consumption is 0.1～5wt%, in the gross weight of pre-polymerization liquid; The consumption of said modified monomer is preferably 1～3wt%, in the gross weight of pre-polymerization liquid.
Described releasing agent is a Triple Pressed Stearic Acid, and its consumption is 0.2～5wt%, in the gross weight of pre-polymerization liquid; The preferred 1.0wt% of described stearic consumption is in the gross weight of pre-polymerization liquid.
Described softening agent is Witcizer 300, o-phthalic acid dibutyl ester, epoxy soybean oil; Described softening agent pref-erable dioctyl phthalate.
Described plasticizer dosage is 0～10wt%, in the gross weight of pre-polymerization liquid; Preferred 3～the 4wt% of plasticizer dosage is in the gross weight of pre-polymerization liquid.
Described initiator is a radical initiator; Comprise peroxide radical initiators such as Lucidol, Di Cumyl Peroxide 99, the peroxo-tert-butyl ester, cyclohexanone peroxide, cyclohexanone peroxide; Azo such as Diisopropyl azodicarboxylate, ABVN type free base initiator; Also comprise colourless Compositional type redox initiation system, like the compound system of methylethyl ketone peroxide-calcium iso-octoate, the composite initiator system that cyclohexanone peroxide-isocaprylic acid potassium is formed.Preferential, select the peroxide initiator for use.
The consumption of described initiator is 0.02～3wt%; Initiator amount is preferably 0.1～0.2wt%, in monomeric gross weight.
Described glass fiber material can preferentially select the continuous glass-fiber felt for transparent glass fibers such as woven fiber glass, continuous glass-fiber felt, chopped glass fiber Nomexs.
The specific refractory power of described glass is between 1.49～1.59.
Described glass is the transparent glass fiber.
The characteristics of described transparent glass fiber are: (a) be the dewaxing glass, promptly fiberglass surfacing does not contain surface treatment agent, though perhaps contain surface treatment agent at first, the glass of surface treatment agent being deviate from fully through the method for high temperature dewaxing or dissolution with solvents; Or the glass of (b) handling through the particular surface treatment agent; The characteristics of this surface treatment agent are to be easy to be dissolved in TEB 3K or the vinylbenzene; As to adopt the unsaturated polyester resin water miscible liquid be main body; Wherein add the surface treatment agent that the A-174 coupling agent is formed, perhaps the surface treatment agent formed of esters of acrylic acid coupling agent.The surface treatment agent of this glass is easy to be dissolved in the steeping fluid, and is preferential, the spun glass of selecting for use the esters of acrylic acid surface treatment agent to handle.
Can find out that from above technical scheme the present invention has following beneficial effect:
The present invention is through regulating the specific refractory power that TEB 3K and cinnamic ratio are regulated resin, and specific refractory power can be regulated in the 1.49-1.59 scope, applicable to the printing opacity glass in the overwhelming majority.
The transmittance of used resin system is very high, and the transmittance of virgin resin can be up to 91%.
Adopt prepolymerized method to prepare steeping fluid, the viscosity of steeping fluid can freely be controlled, and is fine to the dipping effect of glass, in the transparent glass steel of moulding, utilizes the visual existence that can not observe glass, and transmittance is the highest accomplishes 90%.
Crosslinking reaction does not take place in the solidification process, and what obtain is fiber glass reinforced thermoplastics's sheet material, can change its shape after the heating, can finalize the design through second-heating for changing shape, and preparation has the board product of certain curved surface.
Embodiment
Further specify characteristics of the present invention through specific embodiment below.
Embodiment 1:
Glass adopts common commercially available printing opacity alkali-free glass fiber cloth, and area density is 400g/m
2, its specific refractory power is 1.5460.
(1) preparation of prepolymerization liquid:
1000 gram TEB 3Ks, 1300 gram vinylbenzene, 30 gram SY-Monomer Gs, 30 gram Triple Pressed Stearic Acid, 40 gram o-phthalic acid dibutyl esters are mixed; Add 2.6 gram Lucidols, be warming up to 70 ℃, react after 4 hours; Be cooled to normal temperature, gained pre-polymerization liquid is for use.
(2) impregnated glass fiber:
Mould laying glass cloth being used for preparing 3 mm thick sheet materials floods matched moulds with pre-polymerization liquid.
(3) molded curing:
Mould is placed on the thermocompressor, and the mould temperature is arranged on 80 ℃, and Procuring was pressurizeed and is warming up to 120 ℃ and carry out completely solidified after 2 hour.
(4) polishing burr, periphery is repaiied directly:
After half a hour mould is taken off, treat to take off reinforced plastic plate after the mold cools down, utilize emery wheel that periphery is polished, repaiied directly, can obtain high translucent glass fibre board material.
Utilize transmittance mist degree determinator to measure, the transmittance of this 3mm heavy sheet glass steel board is 85%.
Embodiment 2:
Glass adopts the pure white printing opacity alkali-free glass fiber continuous felt of dewaxing, and area density is 200g/m
2, its specific refractory power is 1.560.
(1) preparation of prepolymerization liquid:
1000 gram TEB 3Ks, 2300 gram vinylbenzene, 35 gram SY-Monomer Gs, 35 gram Triple Pressed Stearic Acid, 38 gram o-phthalic acid dibutyl esters are mixed; Add 3.3 gram Lucidols, be warming up to 80 ℃, react after 3 hours; Be cooled to normal temperature, gained pre-polymerization liquid is for use.
(2) impregnated glass fiber:
Mould laying glass cloth being used for preparing 3 mm thick sheet materials floods matched moulds with pre-polymerization liquid.
(3) molded curing:
Mould is placed on the thermocompressor, and the mould temperature is arranged on 80 ℃, and Procuring was pressurizeed and is warming up to 120 ℃ and thoroughly solidify after 2 hour.
(4) polishing burr, periphery is repaiied directly:
After half a hour mould is taken off, treat to take off reinforced plastic plate after the mold cools down, utilize emery wheel that periphery is polished, repaiied directly, can obtain high translucent glass fibre board material.
Utilize transmittance mist degree determinator to measure, the transmittance of this 3mm heavy sheet glass steel board is 89%.
Embodiment 3:
Glass adopts the pure white printing opacity alkali-free glass fiber continuous felt (with embodiment 2) of dewaxing, and area density is 200g/m
2, its specific refractory power is 1.560.
(1) preparation of prepolymerization liquid:
1000 gram TEB 3Ks, 2290 gram vinylbenzene, 35 gram SY-Monomer Gs, 35 gram Triple Pressed Stearic Acid, 30 gram epoxy soybean oils are mixed; Add 3.0 gram cyclohexanone peroxides, be warming up to 60 ℃, react after 16 hours; Be cooled to normal temperature, gained pre-polymerization liquid is for use.
(2) impregnated glass fiber:
Mould laying glass cloth being used for preparing 3 mm thick sheet materials floods with pre-polymerization liquid.Matched moulds.
(3) molded curing:
Mould is placed on the thermocompressor, and the mould temperature is arranged on 80 ℃, and Procuring was pressurizeed and is warming up to 120 ℃ and thoroughly solidify after 2 hour.
(4) polishing burr, periphery is repaiied directly:
After half a hour mould is taken off, treat to take off reinforced plastic plate after the mold cools down, utilize emery wheel that periphery is polished, repaiied directly, can obtain high translucent glass fibre board material.
Utilize transmittance mist degree determinator to measure, the transmittance of this 3mm heavy sheet glass steel board is 89%.
Embodiment 4:
Adopt a kind of pure white medium-alkali glass fibre continuous felt of dewaxing, its specific refractory power is 1.516.
(1) preparation of prepolymerization liquid:
1000 gram TEB 3Ks, 287 gram vinylbenzene, 15 gram maleic anhydrides, 15 gram Triple Pressed Stearic Acid, 20 gram o-phthalic acid dibutyl esters are mixed; Add 1.3 gram Lucidols, be warming up to 85 ℃, react after 2.5 hours; Be cooled to room temperature, gained pre-polymerization liquid is for use.
(2) impregnated glass fiber:
Mould laying glass felt being used for preparing 3 mm thick sheet materials floods matched moulds with pre-polymerization liquid.
(3) molded curing:
Mould is placed on the thermocompressor, and the mould temperature is arranged on 80 ℃, and Procuring was pressurizeed and is warming up to 120 ℃ and thoroughly solidify after 2 hour.
(4) polishing burr, periphery is repaiied directly:
After half a hour mould is taken off, treat to take off reinforced plastic plate after the mold cools down, utilize emery wheel that periphery is polished, repaiied directly, can obtain high translucent glass fibre board material.
Utilize transmittance mist degree determinator to measure, the transmittance of this 3mm heavy sheet glass steel board is 90%.
Embodiment 5:
Adopt a kind of pure white medium-alkali glass fibre continuous felt (with embodiment 4) of dewaxing, its specific refractory power is 1.516.
(1) preparation of prepolymerization liquid:
1000 gram TEB 3Ks, 280 gram vinylbenzene, 15 gram maleic anhydrides, 15 gram Triple Pressed Stearic Acid, 20 gram epoxy soybean oils are mixed, add 2.0 gram Diisopropyl azodicarboxylates, be warming up to 70 ℃, react after 8 hours, be cooled to room temperature, gained pre-polymerization liquid is for use.
(2) impregnated glass fiber:
Mould laying glass felt being used for preparing 3 mm thick sheet materials floods matched moulds with pre-polymerization liquid.
(3) molded curing:
Mould is placed on the thermocompressor, and the mould temperature is arranged on 80 ℃, and Procuring was pressurizeed and is warming up to 120 ℃ and thoroughly solidify after 2 hour.
(4) polishing burr, periphery is repaiied directly:
After half a hour mould is taken off, treat to take off reinforced plastic plate after the mold cools down, utilize emery wheel that periphery is polished, repaiied directly, can obtain high translucent glass fibre board material.
Utilize transmittance mist degree determinator to measure, the transmittance of this 3mm heavy sheet glass steel board is 90%.
The above-mentioned description to embodiment is can understand and use the present invention for ease of the those of ordinary skill of this technical field.The personnel of skilled obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (8)
1. the method for manufacture of one kind high printing opacity fiber glass reinforced thermoplastics sheet material is characterized in that: comprise step:
(1) preparation of pre-polymerization liquid:
TEB 3K, vinylbenzene and modified monomer are mixed according to the certainweight ratio, add releasing agent, softening agent, initiator, start and stir, in polymeric kettle, carry out radical polymerization, treat that viscosity obviously begins to rise after, reduce to room temperature, pre-polymerization liquid;
(2) impregnated glass fiber:
Glass fiber material successively is laid in the mould, successively floods with pre-polymerization liquid, then matched moulds;
(3) molded curing:
At a certain temperature, forming mould is placed on carries out compression molding on the press, until completely solidified;
(4) polishing burr, periphery is repaiied directly:
After the completely solidified, take out reinforced plastic plate, utilize emery wheel that burr are polished smooth, can obtain the translucent glass fibre board material.
2. method according to claim 1 is characterized in that: the temperature of described polymerization reaction kettle is 50～90 ℃; The described pre-polymerization time is 1～16 hour; The viscosity of described pre-polymerization liquid is no more than 0.1Pa.S, and described mould temperature control is at 60～120 ℃.
3. method according to claim 1; It is characterized in that: described TEB 3K and cinnamic weight ratio are decided by the specific refractory power of used glass, make the error of specific refractory power of specific refractory power and the glass of formed polymkeric substance after the complete polymerization of pre-polymerization liquid be no more than 0.1%.
4. method according to claim 1 is characterized in that: described modified monomer is SY-Monomer G or maleic anhydride, and consumption is 0.1～5wt%, in the gross weight of pre-polymerization liquid.
5. method according to claim 1 is characterized in that: described releasing agent is a Triple Pressed Stearic Acid, and its consumption is 0.2～5wt%, in the gross weight of pre-polymerization liquid.
6. method according to claim 1 is characterized in that: described softening agent is Witcizer 300, o-phthalic acid dibutyl ester or epoxy soybean oil; Described plasticizer dosage is 0～10wt%, in the gross weight of pre-polymerization liquid.
7. method according to claim 1; It is characterized in that: described initiator is a radical initiator, comprises the compound system of Lucidol, Di Cumyl Peroxide 99, the peroxo-tert-butyl ester, cyclohexanone peroxide, cyclohexanone peroxide, Diisopropyl azodicarboxylate, ABVN, methylethyl ketone peroxide-calcium iso-octoate or the composite initiator system that cyclohexanone peroxide-isocaprylic acid potassium is formed; The consumption of described initiator is 0.02～3wt%, in monomeric gross weight.
8. method according to claim 1 is characterized in that: described glass fiber material is woven fiber glass, continuous glass-fiber felt or chopped glass fiber Nomex; The specific refractory power of described glass is between 1.49～1.59; Described glass is the transparent glass fiber.
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| CN108102273A (en) * | 2017-12-25 | 2018-06-01 | 温州中祥光电科技发展有限公司 | A kind of high tenacity acryl plates and preparation method thereof |
| CN108495866A (en) * | 2015-12-28 | 2018-09-04 | 雅马哈株式会社 | Resin combination, FRP sheet materials and shaped article for FRP |
| CN108587057A (en) * | 2018-04-10 | 2018-09-28 | 安徽宏志建材科技有限公司 | A kind of daylighting weather-resistant composite, plane skylight and preparation method thereof |
| GB2575746A (en) * | 2017-02-02 | 2020-01-22 | Fire Curtains Inc | Flexible translucent to transparent fireproof composite material |
| CN111978459A (en) * | 2019-05-24 | 2020-11-24 | 汉能移动能源控股集团有限公司 | PMMA/glass fiber composite material and preparation method and application thereof |
| CN112063088A (en) * | 2019-05-24 | 2020-12-11 | 汉能移动能源控股集团有限公司 | PMMA/glass fiber composite material and preparation method and application thereof |
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| US10876002B2 (en) | 2015-12-28 | 2020-12-29 | Yamaha Corporation | Resin composition for FRP, FRP sheet and molded product |
| CN108495866A (en) * | 2015-12-28 | 2018-09-04 | 雅马哈株式会社 | Resin combination, FRP sheet materials and shaped article for FRP |
| CN108495866B (en) * | 2015-12-28 | 2021-03-02 | 雅马哈株式会社 | Resin composition for FRP, FRP sheet and molded product |
| US10695795B2 (en) | 2017-02-02 | 2020-06-30 | Fire Curtains, Inc. | Method of producing a composite panel |
| GB2559633B (en) * | 2017-02-02 | 2020-02-19 | Fire Curtains Inc | Flexible translucent to transparent fireproof composite material |
| GB2576439A (en) * | 2017-02-02 | 2020-02-19 | Fire Curtains Inc | Flexible translucent to transparent fireproof composite material |
| GB2576439B (en) * | 2017-02-02 | 2020-07-15 | Fire Curtains Inc | Flexible translucent to transparent fireproof composite material |
| GB2575746B (en) * | 2017-02-02 | 2020-12-09 | Fire Curtains Inc | Flexible translucent to transparent fireproof composite material |
| GB2575746A (en) * | 2017-02-02 | 2020-01-22 | Fire Curtains Inc | Flexible translucent to transparent fireproof composite material |
| CN108102273A (en) * | 2017-12-25 | 2018-06-01 | 温州中祥光电科技发展有限公司 | A kind of high tenacity acryl plates and preparation method thereof |
| CN108587057A (en) * | 2018-04-10 | 2018-09-28 | 安徽宏志建材科技有限公司 | A kind of daylighting weather-resistant composite, plane skylight and preparation method thereof |
| CN111978459A (en) * | 2019-05-24 | 2020-11-24 | 汉能移动能源控股集团有限公司 | PMMA/glass fiber composite material and preparation method and application thereof |
| CN112063088A (en) * | 2019-05-24 | 2020-12-11 | 汉能移动能源控股集团有限公司 | PMMA/glass fiber composite material and preparation method and application thereof |
| CN113549170A (en) * | 2020-04-23 | 2021-10-26 | 西安昊锐电子科技有限公司 | Backing plate for cutting solar silicon wafer and manufacturing method thereof |
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Denomination of invention: Method for preparing transparent thermoplastic glass fiber reinforced plastic sheet Effective date of registration: 20191202 Granted publication date: 20140604 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980000815 |
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