CN102558701B - 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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- CN102558701B CN102558701B CN201010580639.3A CN201010580639A CN102558701B CN 102558701 B CN102558701 B CN 102558701B CN 201010580639 A CN201010580639 A CN 201010580639A CN 102558701 B CN102558701 B CN 102558701B
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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 glass fibre reinforced plastics technology field, relate to a kind of preparation method of reinforced plastic plate.
Background technology
Transparent glass steel is a kind of galss fiber reinforced resin based composites, not only has the high strength of glass reinforced plastic, the feature of high-modulus, and has good light transmission, can be used as the construction of lighting material for transparent square, transparent worker-house, transparent green house of vegetables.Conventionally, transparent grp is to adopt the compound and preparation of thermosetting resin and glass fibre, once shortcoming be glass reinforced plastic and shape, can not change shape by heating again, do not possess the ability of secondary temperature distortion, and be difficult to recycling.In addition,, due to the inherent defect of thermosetting resin, the shock resistance of thermoset transparent glass steel is 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 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 production 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 glass fibre to carry out pultrusion, produce continuous section bar.Because the melt viscosity of polymkeric substance is very large, a significant shortcoming of the method is in pultrusion process, and the organic fibre of melting is difficult to glass fibre thorough impregnation, and this can have influence on the light transmission of product.
Summary of the invention
The object of the invention is to for the defect of prior art and a kind of printing opacity fiber glass reinforced thermoplastics preparation of plates method is provided.
The present invention is by the following technical solutions:
Key problem in technology of the present invention is that requirement resin matrix and glass specific refractory power are wanted matched, makes the error of the specific refractory power of resin matrix and glass be 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 above formula:
N
(PMMA)for the specific refractory power of pure polymethylmethacrylate (PMMA), this value gets 1.490;
W%
(PMMA)for the weight ratio of PMMA in multipolymer;
N
(PS)for the specific refractory power of pure polystyrene (PS), this value gets 1.591.
W%
(PS)for the weight ratio of PS in multipolymer;
Utilize the monomer ratio that above formula calculates can only roughly determine a scope, also to consider the impact on resin specific refractory power of modified monomer, releasing agent and softening agent, because of the specific refractory power of releasing agent, softening agent and modified monomer lower, add these auxiliary agents can reduce to a certain extent the specific refractory power of resin matrix, therefore in actual formula, should suitably strengthen cinnamic consumption.
Concrete grammar is: first by calculating rough determine methyl methacrylate and cinnamic proportioning, then add modified monomer, initiator, releasing agent, softening agent is also fixed the consumption of these auxiliary agents, carry out radical polymerization, after question response is complete, utilize Abbe refractometer to measure the specific refractory power of resulting polymers, if gained specific refractory power is lower than the specific refractory power of glass, suitably increase cinnamic consumption, if gained specific refractory power is higher than the specific refractory power of glass, suitably reduce cinnamic consumption, until the specific refractory power error of the specific refractory power of resinous substrates and glass is lower than 0.1%.
A manufacture method for high printing opacity fiber glass reinforced thermoplastics sheet material, comprises step:
(1) preparation of pre-polymerization liquid:
Methyl methacrylate, vinylbenzene and modified monomer are mixed according to certainweight ratio, add releasing agent, softening agent, initiator, start and stir, in polymeric kettle, carry out radical polymerization, after viscosity obviously starts to rise, be down to room temperature, obtain pre-polymerization liquid;
(2) impregnated glass fiber:
Glass fiber material is successively laid in mould, successively floods then matched moulds with pre-polymerization liquid;
(3) molded curing:
At a certain temperature, forming mould is placed on press and carries out compression molding, until completely curing;
(4) polishing burr, periphery is repaiied directly:
After solidifying completely, take out reinforced plastic plate, utilize emery wheel that burr are polished smooth, can obtain 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 methyl methacrylate and cinnamic weight ratio are determined by the specific refractory power of glass used, make the specific refractory power of polymkeric substance that forms after the complete polymerization of pre-polymerization liquid and the error of the specific refractory power of glass be no more than 0.1%.
Described modified monomer is glycidyl methacrylate or maleic anhydride, and consumption is 0.1～5wt%, in the gross weight of pre-polymerization liquid; The consumption of described modified monomer is preferably 1～3wt%, in the gross weight of pre-polymerization liquid.
Described releasing agent is stearic acid, and its consumption is 0.2～5wt%, in the gross weight of pre-polymerization liquid; The described preferred 1.0wt% of stearic consumption, in the gross weight of pre-polymerization liquid.
Described softening agent is dibutyl phthalate, o-phthalic acid dibutyl ester, epoxy soybean oil; Described softening agent pref-erable dioctyl phthalate.
The consumption of described softening agent is 0～10wt%, in the gross weight of pre-polymerization liquid; Preferably 3～4wt% of the consumption of softening agent, in the gross weight of pre-polymerization liquid.
Described initiator is radical initiator, comprise the peroxide radical initiators such as benzoyl peroxide, dicumyl peroxide, the peroxidation tert-butyl ester, cyclohexanone peroxide, cyclohexanone peroxide, the azo such as Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile) radical initiator, also comprise colourless Compositional type redox initiation system, as the composite initiator system of the compound system of methylethyl ketone peroxide-calcium iso-octoate, cyclohexanone peroxide-isocaprylic acid potassium composition.Preferential, select peroxide initiator.
The consumption of described initiator is 0.02～3wt%; Initiator amount is preferably 0.1～0.2wt%, in the gross weight of monomer.
Described glass fiber material can be the transparent glass fibers such as woven fiber glass, continuous glass-fiber felt, chopped glass fiber Nomex, preferentially selects continuous glass-fiber felt.
The specific refractory power of described glass is between 1.49～1.59.
Described glass is transparent glass fiber.
The feature of described transparent glass fiber is: be (a) dewaxing glass, be that fiberglass surfacing is not containing surface treatment agent, although or contain at first surface treatment agent, by the glass that high temperature dewaxes or the method for dissolution with solvents is deviate from surface treatment agent completely; Or (b) through the glass of particular surface treatment agent processing, the feature of this surface treatment agent is to be easy to be dissolved in methyl methacrylate or vinylbenzene, as to adopt unsaturated polyester resin water miscible liquid be main body, the surface treatment agent that wherein adds A-174 coupling agent to form, or the surface treatment agent that forms of esters of acrylic acid coupling agent.The surface treatment agent of this glass is easy to be dissolved in steeping fluid, preferential, selects the glass fibre of esters of acrylic acid surface treatment agent processing.
As can be seen from the above technical solutions, the present invention has following beneficial effect:
The present invention is by regulating methyl methacrylate and cinnamic ratio to regulate the specific refractory power of resin, and specific refractory power can regulate within the scope of 1.49-1.59, applicable to the printing opacity glass most.
The transmittance of resin system used 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, 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 occur in solidification process, and what obtain is fiber glass reinforced thermoplastics's sheet material, after heating, can change its shape, can shape to change shape by second-heating, and preparation has the board product of certain curved surface.
Embodiment
Further illustrate feature of the present invention below by specific embodiment.
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 grams of methyl methacrylates, 1300 grams of vinylbenzene, 30 grams of glycidyl methacrylate, 30 grams of stearic acid, 40 grams of o-phthalic acid dibutyl esters are mixed, add 2.6 grams of benzoyl peroxides, be warming up to 70 ℃, react after 4 hours, be cooled to normal temperature, gained pre-polymerization liquid is stand-by.
(2) impregnated glass fiber:
In the mould for the preparation of 3 mm thick sheet materials, lay glass-fiber-fabric, flood matched moulds with pre-polymerization liquid.
(3) molded curing:
Mould is placed on thermocompressor, and mould temperature is arranged on 80 ℃, and Procuring, after 2 hours, is pressurizeed and is warming up to 120 ℃ and solidify completely.
(4) polishing burr, periphery is repaiied directly:
After half an hour, mould is taken off, after mold cools down, take off reinforced plastic plate, 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 grams of methyl methacrylates, 2300 grams of vinylbenzene, 35 grams of glycidyl methacrylate, 35 grams of stearic acid, 38 grams of o-phthalic acid dibutyl esters are mixed, add 3.3 grams of benzoyl peroxides, be warming up to 80 ℃, react after 3 hours, be cooled to normal temperature, gained pre-polymerization liquid is stand-by.
(2) impregnated glass fiber:
In the mould for the preparation of 3 mm thick sheet materials, lay glass-fiber-fabric, flood matched moulds with pre-polymerization liquid.
(3) molded curing:
Mould is placed on thermocompressor, and mould temperature is arranged on 80 ℃, and Procuring, after 2 hours, is pressurizeed and is warming up to 120 ℃ and thoroughly solidify.
(4) polishing burr, periphery is repaiied directly:
After half an hour, mould is taken off, after mold cools down, take off reinforced plastic plate, 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 grams of methyl methacrylates, 2290 grams of vinylbenzene, 35 grams of glycidyl methacrylate, 35 grams of stearic acid, 30 grams of epoxy soybean oils are mixed, add 3.0 grams of cyclohexanone peroxides, be warming up to 60 ℃, react after 16 hours, be cooled to normal temperature, gained pre-polymerization liquid is stand-by.
(2) impregnated glass fiber:
In the mould for the preparation of 3 mm thick sheet materials, lay glass-fiber-fabric, flood with pre-polymerization liquid.Matched moulds.
(3) molded curing:
Mould is placed on thermocompressor, and mould temperature is arranged on 80 ℃, and Procuring, after 2 hours, is pressurizeed and is warming up to 120 ℃ and thoroughly solidify.
(4) polishing burr, periphery is repaiied directly:
After half an hour, mould is taken off, after mold cools down, take off reinforced plastic plate, 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:
The pure white medium-alkali glass fibre continuous felt that adopts a kind of dewaxing, its specific refractory power is 1.516.
(1) preparation of prepolymerization liquid:
1000 grams of methyl methacrylates, 287 grams of vinylbenzene, 15 grams of maleic anhydrides, 15 grams of stearic acid, 20 grams of o-phthalic acid dibutyl esters are mixed, add 1.3 grams of benzoyl peroxides, be warming up to 85 ℃, react after 2.5 hours, be cooled to room temperature, gained pre-polymerization liquid is stand-by.
(2) impregnated glass fiber:
In the mould for the preparation of 3 mm thick sheet materials, lay Chopped Strand Mat, flood matched moulds with pre-polymerization liquid.
(3) molded curing:
Mould is placed on thermocompressor, and mould temperature is arranged on 80 ℃, and Procuring, after 2 hours, is pressurizeed and is warming up to 120 ℃ and thoroughly solidify.
(4) polishing burr, periphery is repaiied directly:
After half an hour, mould is taken off, after mold cools down, take off reinforced plastic plate, 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:
The pure white medium-alkali glass fibre continuous felt (with embodiment 4) that adopts a kind of dewaxing, its specific refractory power is 1.516.
(1) preparation of prepolymerization liquid:
1000 grams of methyl methacrylates, 280 grams of vinylbenzene, 15 grams of maleic anhydrides, 15 grams of stearic acid, 20 grams of epoxy soybean oils are mixed, add 2.0 grams of Diisopropyl azodicarboxylates, be warming up to 70 ℃, react after 8 hours, be cooled to room temperature, gained pre-polymerization liquid is stand-by.
(2) impregnated glass fiber:
In the mould for the preparation of 3 mm thick sheet materials, lay Chopped Strand Mat, flood matched moulds with pre-polymerization liquid.
(3) molded curing:
Mould is placed on thermocompressor, and mould temperature is arranged on 80 ℃, and Procuring, after 2 hours, is pressurizeed and is warming up to 120 ℃ and thoroughly solidify.
(4) polishing burr, periphery is repaiied directly:
After half an hour, mould is taken off, after mold cools down, take off reinforced plastic plate, 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 apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.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 departing from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (4)
1. a manufacture method for high printing opacity fiber glass reinforced thermoplastics sheet material, is characterized in that: comprise step:
(1) preparation of pre-polymerization liquid:
Methyl methacrylate, vinylbenzene and modified monomer are mixed according to certainweight ratio, add releasing agent, softening agent, initiator, start and stir, in polymeric kettle, carry out radical polymerization, after viscosity obviously starts to rise, be down to room temperature, obtain pre-polymerization liquid; The viscosity of described pre-polymerization liquid is no more than 0.1Pa.s;
(2) impregnated glass fiber:
Glass fiber material is successively laid in mould, successively floods then matched moulds with pre-polymerization liquid;
(3) molded curing:
At a certain temperature, forming mould is placed on press and carries out compression molding, until completely curing;
(4) polishing burr, periphery is repaiied directly:
After solidifying completely, take out reinforced plastic plate, utilize emery wheel that burr are polished smooth, can obtain translucent glass fibre board material;
Described modified monomer is glycidyl methacrylate or maleic anhydride, and consumption is 0.1～5wt%, in the gross weight of pre-polymerization liquid;
Described releasing agent is stearic acid, and its consumption is 0.2～5wt%, in the gross weight of pre-polymerization liquid;
Described softening agent is dibutyl phthalate, o-phthalic acid dibutyl ester or epoxy soybean oil; The consumption of described softening agent is 0～10wt%, in the gross weight of pre-polymerization liquid;
Described initiator is radical initiator, comprises the compound system of benzoyl peroxide, dicumyl peroxide, the peroxidation tert-butyl ester, cyclohexanone peroxide, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), methylethyl ketone peroxide-calcium iso-octoate or the composite initiator system of cyclohexanone peroxide-isocaprylic acid potassium composition; The consumption of described initiator is 0.02～3wt%, in the gross weight of monomer.
2. method according to claim 1, is characterized in that: the temperature of described polymeric kettle is 50～90 ℃; The pre-polymerization time is 1～16 hour; Mould temperature control is at 60～120 ℃.
3. method according to claim 1, it is characterized in that: described methyl methacrylate and cinnamic weight ratio are determined by the specific refractory power of glass used, make the specific refractory power of polymkeric substance that forms after the complete polymerization of pre-polymerization liquid and the error of the specific refractory power of glass be no more than 0.1%.
4. 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 transparent glass fiber.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2559633A (en) * | 2017-02-02 | 2018-08-15 | Bailey Douglas | Flexible translucent to transparent fireproof composite material |
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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 |
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| 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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| CN1006711B (en) * | 1985-08-07 | 1990-02-07 | 日本触媒化学工业株式会社 | Curable composition method for manufacture thereof and uses thereof |
| CN1315463A (en) * | 2000-03-30 | 2001-10-03 | 上海杰事杰新材料股份有限公司 | Composite resin/fibre material and its preparing process |
| CN1162469C (en) * | 2002-07-01 | 2004-08-18 | 康艳红 | Full-transparency solidifying material for non-alkali cloth reinforced plastics |
| CN101131033A (en) * | 2006-08-25 | 2008-02-27 | 江苏九鼎新材料股份有限公司 | Transparent glass fibre reinforced plastic grille and manufacturing method thereof |
| CN101358023A (en) * | 2007-08-01 | 2009-02-04 | 上海麦登复合材料有限公司 | Transparent anti static flame-retardant glass fibre reinforced plastic material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2559633A (en) * | 2017-02-02 | 2018-08-15 | Bailey Douglas | Flexible translucent to transparent fireproof composite material |
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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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