CN100564448C - A kind of method for preparing molded epoxy resin sheet and products thereof - Google Patents
A kind of method for preparing molded epoxy resin sheet and products thereof Download PDFInfo
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- CN100564448C CN100564448C CNB2007100526835A CN200710052683A CN100564448C CN 100564448 C CN100564448 C CN 100564448C CN B2007100526835 A CNB2007100526835 A CN B2007100526835A CN 200710052683 A CN200710052683 A CN 200710052683A CN 100564448 C CN100564448 C CN 100564448C
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Abstract
The method for preparing molded epoxy resin sheet provided by the invention is: adopt the binary isocyanate compound to the thickening of blending epoxy system, chopped strand strengthens, and overlay film is prepared into the tack-free molded epoxy resin sheet of shearing; This method comprises the preparation of epoxy paste, the preparation and the maturation stage of molded epoxy resin sheet.This molded epoxy resin sheet, core is by having flooded the fibrous of epoxy paste in the middle of it, upper and lower surface covers with the PE film; Meter is made by following raw material: 100 parts of blending epoxies, 4～10 parts of thinners, 15～80 parts in solidifying agent, 5～20 parts of thickening materials, 1～4 part of inner pattern releasing agent applicable, 80～180 parts of fillers, 50～150 parts of fibers by weight.This molded epoxy resin sheet has advantages such as the heat flow performance is good, set time short, the storage time is long, corrosion-resistant, and preparation technology is simple.Can prepare the higher epoxy composite material structure unit of intensity by hot-press solidifying.
Description
Technical field
The present invention relates to the material field, particularly relate to a kind of method for preparing molded epoxy resin sheet and products thereof.
Background technology
Die press technology for forming is a kind of important composite material process planning, and sheet molding compound SMC (sheet moldingcompound) is the important formed material of mould pressing process.Its middle core of SMC is made up of the glass fibre that has soaked into resin paste, and upper and lower surface covers with the PE film; Resin paste is made up of unsaturated polyester, low shrinkage additive, solidifying agent, thickening material, inner pattern releasing agent applicable, filler, makes sheet material through SMC pelleter impregnated glass fiber, carries out rolling again, passes through thickening then, reaches tack-free state, is used for compression molding.The SMC sheet material is the molding compound that a kind of dry method that grows up the sixties in 20th century is made fibre reinforced plastics, through 40 years of development, the SMC die press technology for forming now progressively develops into the most ripe in the field of compound material, a kind of very widely technology of application, its product is widely used in fields such as building, automobile, electronics/electric, this technology has advantages such as mechanization degree height, production efficiency height, constant product quality, production cost be low, makes it become a kind of important moulding process of glass reinforced plastic industry rapidly.
SMC mainly is to be matrix (seldom part Vinylite) with the unsaturated polyester resin at present, yet this unsaturated polyester resin SMC exists as temperature tolerance, erosion resistance, insulation effect relatively poor relatively, shortcomings such as structural strength is lower can not be applied to the occasion that some has property to require.
The Chinese patent publication number is that the patent " preparation method of reinforced epoxy moulding compound for packaging electric equipment " of CN1150597A provides prescription and the preparation method of a kind of electrical equipment encapsulation with glass fiber reinforcement epoxy molding compound, this epoxy molding plastic is by the kneading of heating through in advance of Resins, epoxy and solidifying agent, filler, releasing agent, cooling, pulverizing are expected as (A); Solidifying agent and filler, curing catalyst, are expected as (B) through cooling, pulverizing through the kneading of heating; Material is mixing on the heating roller with (A) with (B), and adds short glass fiber, tinting material, makes sheet or pie finished product.This patent only is to adopt mixing method to make a kind of sheet or the electric encapsulation epoxy molding plastic of pie, does not relate to the thickening of Resins, epoxy and the preparation of molded epoxy resin sheet in the preparation process.
Existing glass fiber reinforcement epoxy molding compound major applications on Electronic Packaging, though have it is made sheet, what its adopted is mixing method, does not adopt the method for chemical thickening compression molding, is not molded epoxy resin sheet truly.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method for preparing molded epoxy resin sheet is provided, this method is less demanding, can adopt existing polyester SMC production facility to produce, the molded epoxy resin sheet of being produced is realized the preparation of high-strength epoxy composite structural part by hot press forming technology.
The present invention solves its technical problem by following technical scheme:
The preparation method of molded epoxy resin sheet provided by the invention is: adopt the binary isocyanate compound to the thickening of blending epoxy system, chopped strand strengthens, and overlay film is prepared into the tack-free molded epoxy resin sheet of shearing.
Count by weight, this molded epoxy resin sheet is made by following raw material: 100 parts of blending epoxies, 4～10 parts of thinners, 15～80 parts in solidifying agent, 5～20 parts of thickening materials, 1～4 part of inner pattern releasing agent applicable, 80～180 parts of fillers, 50～150 parts of fibers.Wherein, blending epoxy is made up of for 10～40 parts 60～90 parts of liquid Racemic glycidol ether type epoxies and solid bisphenol A type epoxy resin.Described thickening material is 4,4 '-diphenylmethanediisocyanate, tolylene diisocyanate, 1,4-cyclohexyl diisocyanate, 2, in the 4-dimethylene diisocyanate more than one.
The preparation of this molded epoxy resin sheet specifically is to adopt the method that may further comprise the steps:
(1) preparation of epoxy paste: liquid Racemic glycidol ether type epoxy and solid bisphenol A type epoxy resin are joined in the mixing tank of band heating and heat-insulating device, and heating makes its thorough mixing; Treat that its cooling back joins in the mixing tank in proportion successively by the order of thinner, inner pattern releasing agent applicable, filler, add solidifying agent, thickening material after mixing again, mix and make epoxy paste;
(2) preparation of molded epoxy resin sheet:, epoxy paste evenly is coated on the upper and lower PE film by scraper; Pass through to regulate cutting unit then, cutting fibre, the length of controlling fiber and content, overlay film is about to upper and lower PE film and pastes relatively then, forms the epoxy paste sheet material that a kind of above and below at fiber all is covered with the PE film; Again the epoxy paste sheet material is extruded by roller, its fiber and resin are fully flooded, be shaped to sheet material, carry out rolling then;
(3) slaking of molded epoxy resin sheet: the sheet material of rolling is transported to the thickening of thickening chamber, and the control thickening temperature is 30-60 ℃, and the sheet material thickening time is 24-240 hour, obtains described molded epoxy resin sheet.
Described liquid Racemic glycidol ether type epoxy can be a kind of be that raw material prepares through polycondensation by polyphenol or polyvalent alcohol and epoxy chloropropane, it be in bisphenol A diglycidyl ether, Bisphenol F diglycidylether, the bisphenol-S diglycidyl ether more than one.
Described solid bisphenol A type epoxy resin can adopt molecular weight greater than 900, is solid-state middle and high molecular weight bisphenol A type epoxy resin under the normal temperature.
Described thinner can be in mono-epoxy compounds thinner, the multi-epoxy compounds thinner more than one.
Described solidifying agent can be in aromatic amine, anhydrides, Dyhard RU 100 class, organic hydrazides class, the linear phenolic resin etc. more than one.
Described inner pattern releasing agent applicable can be selected in stearic acid, Zinic stearas, calcium stearate, the Magnesium Stearate etc. more than one for use.
Described filler can be selected in light calcium carbonate, water-ground limestone, aluminium hydroxide, aluminum oxide, kaolin, magnesiumcarbonate, Calucium Silicate powder, silicon-dioxide, the mica etc. more than one for use.
Described fiber can be selected one or more fiber hybrids in glass fibre, carbon fiber, the aramid fiber etc. for use, and its length is 25～60mm.
Molded epoxy resin sheet by method for preparing provided by the invention, for: core is by having flooded the fibrous of epoxy paste in the middle of it, and upper and lower surface covers with the PE film.
The present invention compared with prior art has following major advantage:
One. a kind of long fibre-reinforced technical scheme that is used for the compression molding molded epoxy resin sheet is disclosed, this sheet molding compound prepares difform epoxy construction spare with good mechanical characteristic through hot-forming, be the upgrading products of unsaturated polyester SMC system, be different from traditional used for packing material epoxy molding plastic.
They are two years old. a kind of neo-epoxy resin system thickening mode is disclosed, adopt the thickening of binary isocyanate compound to contain the blending epoxy system of solid bisphenol A type epoxy resin, by the adjusting of addition, thickening temperature and time, effective required viscosity in gate ring epoxy resins and the sheet preparation process thereof.Regulate in can the red-tape operati process tack-freely by viscosity, can guarantee that again resin has good mobility in hot pressing.
They are three years old. excellent product performance: with unsaturated polyester SMC goods mutually specific tenacity significantly improve, corrosion resistance nature and insulating property all strengthen to some extent.Simultaneously, this sheet material also has advantages such as the heat flow performance is good, set time short, the storage time is long, can prepare the higher epoxy composite material structure unit of intensity by hot-press solidifying.
They are four years old. be beneficial to production: can adopt existing polyester SMC production facility to produce.Manufacturing technique requirent is not high, and only needing increases heating and heat-insulating device in the mixing of materials stage.
Embodiment
Molded epoxy resin sheet provided by the invention, its preparation method comprise the preparation of epoxy paste, the preparation of molded epoxy resin sheet and the maturation stage of molded epoxy resin sheet.
Molded epoxy resin sheet provided by the invention, core is by having flooded the fibrous of epoxy paste in the middle of it, upper and lower surface covers with the PE film; Count by weight, this molded epoxy resin sheet is made by following raw material: 100 parts of blending epoxies, 4～10 parts of thinners, 15～80 parts in solidifying agent, 5～20 parts of thickening materials, 1～4 part of inner pattern releasing agent applicable, 80～180 parts of fillers, 50～150 parts of fibers; Wherein, blending epoxy is made up of for 10～40 parts 60～90 parts of liquid Racemic glycidol ether type epoxies and solid bisphenol A type epoxy resin.
Below in conjunction with specific embodiment method provided by the invention is described further, but does not limit the present invention.
Embodiment 1:
1. the preparation of epoxy paste:
Liquid Racemic glycidol ether type epoxy and solid bisphenol A type epoxy resin are joined in the mixing tank of band heating and heat-insulating device, and heating makes its thorough mixing; Treat that its cooling back joins in the mixing tank in proportion successively by the order of thinner, inner pattern releasing agent applicable, filler, add solidifying agent, thickening material after mixing again, mix and make epoxy paste.Count by weight, each proportioning raw materials is: 90 parts of liquid Racemic glycidol ether type epoxies, 10 parts of solid bisphenol A type epoxy resins, 10 parts of thinners, 50 parts in solidifying agent, 5 parts of thickening materials, 4 parts of inner pattern releasing agent applicables, 180 parts of fillers, 150 parts of fibers.
In the above-mentioned prescription, liquid Racemic glycidol ether type epoxy is an epoxy resin E-44, the solid bisphenol A type epoxy resin is E-14, thinner is a phenyl glycidyl ether, solidifying agent is a linear phenolic resin, and thickening material is a tolylene diisocyanate, and inner pattern releasing agent applicable adopts calcium stearate, filler is a light calcium carbonate, and fiber is that its length of alkali free glass fibre is 30-50mm.Can add 1% DMP-30 curing catalyst as Resins, epoxy for the curing speed of accelerating Resins, epoxy.
2. the preparation of molded epoxy resin sheet:
By scraper, epoxy paste evenly is coated on the upper and lower PE film; Again by regulating cutting unit, cutting glass fibre, the length of feed glass fiber and content; Upper and lower PE film is pasted relatively, formed a kind of upper and lower epoxy paste sheet material that all is covered with the PE film; Again the epoxy paste sheet material is extruded by roller, its fiber and resin are fully flooded, be shaped to sheet material, carry out rolling then;
3. the slaking of molded epoxy resin sheet:
The sheet material of rolling is transported to the thickening of thickening chamber, and the temperature of thickening chamber is set to 50 ℃, and the sheet material thickening time is 192 hours, obtains described molded epoxy resin sheet.
Embodiment 2:
In this example, except that each proportioning raw materials had following variation, other was with embodiment 1.
Count by weight, each proportioning raw materials is: 60 parts of liquid Racemic glycidol ether type epoxies, 40 parts of solid bisphenol A type epoxy resins, 4 parts of thinners, 20 parts in solidifying agent, 5 parts of thickening materials, 1 part of inner pattern releasing agent applicable, 80 parts of fillers, 50 parts of fibers.
Embodiment 3:
In this example, except that each proportioning raw materials had following variation, other was with embodiment 1.
Count by weight, each proportioning raw materials is: 75 parts of liquid Racemic glycidol ether type epoxies, 25 parts of solid bisphenol A type epoxy resins, 7 parts of thinners, 40 parts in solidifying agent, 12.5 parts of thickening materials, 2.5 parts of inner pattern releasing agent applicables, 130 parts of fillers, 100 parts of fibers.
Embodiment 4:
In this example, except that each proportioning raw materials had following variation, other was with embodiment 1.
Count by weight, each proportioning raw materials is: 70 parts of liquid Racemic glycidol ether type epoxies, 30 parts of solid bisphenol A type epoxy resins, 5 parts of thinners, 30 parts in solidifying agent, 10 parts of thickening materials, 2 parts of inner pattern releasing agent applicables, 100 parts of fillers, 70 parts of fibers.
Embodiment 5:
The molded epoxy resin sheet that this example provides in the middle of it core be by having flooded the fibrous of epoxy paste, upper and lower surface covers with the PE film, it prepare the method that employing may further comprise the steps:
1. the preparation of epoxy paste:
Liquid Racemic glycidol ether type epoxy and solid bisphenol A type epoxy resin are joined in the mixing tank of band heating and heat-insulating device, and heating makes its thorough mixing; Treat that its cooling back joins in the mixing tank in proportion successively by the order of thinner, inner pattern releasing agent applicable, filler, add solidifying agent, thickening material after mixing again, mix and make epoxy paste.Count by weight, each proportioning raw materials is: 80 parts of liquid Racemic glycidol ether type epoxies, 20 parts of solid bisphenol A type epoxy resins, 6 parts of thinners, 15 parts in solidifying agent, 12 parts of thickening materials, 3 parts of inner pattern releasing agent applicables, 120 parts of fillers, 100 parts of fibers.
In the above-mentioned prescription, liquid Racemic glycidol ether type epoxy is Resins, epoxy E-51, the solid bisphenol A type epoxy resin is E-06, and thinner adopts glycidyl allyl ether, and solidifying agent adopts wherein mphenylenediamine and 4 of low melting eutectics mixing aromatic amine, the ratio of 4 '-diaminodiphenyl-methane is 1: 1, thickening material adopts 4, the 4-diphenylmethanediisocyanate, and inner pattern releasing agent applicable adopts Zinic stearas, filler adopts aluminium hydroxide, and it is 35-55mm that fiber adopts its length of carbon fiber.
2. the preparation of molded epoxy resin sheet: with embodiment 1.
3. the slaking of molded epoxy resin sheet:
This step is 240 hours except that the temperature of thickening chamber is set to 40 ℃, sheet material thickening time, and other is with embodiment 1.
Embodiment 6:
In this example, except that each proportioning raw materials had following variation, other was with embodiment 5.
Count by weight, each proportioning raw materials is: 85 parts of liquid Racemic glycidol ether type epoxies, 15 parts of solid bisphenol A type epoxy resins, 6 parts of thinners, 17.5 parts in solidifying agent, 7 parts of thickening materials, 2 parts of inner pattern releasing agent applicables, 130 parts of fillers, 90 parts of fibers.
Embodiment 7:
In this example, except that each proportioning raw materials had following variation, other was with embodiment 5.
Count by weight, each proportioning raw materials is: 90 parts of liquid Racemic glycidol ether type epoxies, 10 parts of solid bisphenol A type epoxy resins, 9 parts of thinners, 19 parts in solidifying agent, 15 parts of thickening materials, 3 parts of inner pattern releasing agent applicables, 150 parts of fillers, 120 parts of fibers.
Embodiment 8:
In this example, except that each proportioning raw materials had following variation, other was with embodiment 5.
Count by weight, each proportioning raw materials is: 65 parts of liquid Racemic glycidol ether type epoxies, 35 parts of solid bisphenol A type epoxy resins, 7 parts of thinners, 15 parts in solidifying agent, 18 parts of thickening materials, 3 parts of inner pattern releasing agent applicables, 180 parts of fillers, 150 parts of fibers.
Embodiment 9:
The molded epoxy resin sheet that this example provides in the middle of it core be by having flooded the fibrous of epoxy paste, upper and lower surface covers with the PE film, it prepare the method that employing may further comprise the steps:
1. the preparation of epoxy paste:
Liquid Racemic glycidol ether type epoxy and solid bisphenol A type epoxy resin are joined in the mixing tank of band heating and heat-insulating device, and heating makes its thorough mixing; Treat that its cooling back joins in the mixing tank in proportion successively by the order of thinner, inner pattern releasing agent applicable, filler, add solidifying agent, thickening material after mixing again, mix and make epoxy paste.Count by weight, each proportioning raw materials is: 65 parts of liquid Racemic glycidol ether type epoxies, 35 parts of solid bisphenol A type epoxy resins, 10 parts of thinners, 60 parts in solidifying agent, 11 parts of thickening materials, 4 parts of inner pattern releasing agent applicables, 120 parts of fillers, 120 parts of fibers.
In the above-mentioned prescription, liquid Racemic glycidol ether type epoxy is Resins, epoxy E-42, the solid bisphenol A type epoxy resin is E-12, solidifying agent adopts methyl tetrahydrophthalic anhydride, thickening material adopts 2, the 4-dimethylene diisocyanate, and inner pattern releasing agent applicable adopts calcium stearate, filler adopts light calcium carbonate, and it is 30-45mm that fiber adopts its length of alkali free glass fibre.Can add 1% DMP-30 curing catalyst as Resins, epoxy for the curing speed of accelerating Resins, epoxy.
2. the preparation of molded epoxy resin sheet: with embodiment 1.
3. the slaking of molded epoxy resin sheet:
This step is 120 hours except that the temperature of thickening chamber is set to 60 ℃, sheet material thickening time, and other is with embodiment 1.
Embodiment 10:
In this example, except that each proportioning raw materials had following variation, other was with embodiment 9.
Count by weight, each proportioning raw materials is: 90 parts of liquid Racemic glycidol ether type epoxies, 10 parts of solid bisphenol A type epoxy resins, 10 parts of thinners, 80 parts in solidifying agent, 11 parts of thickening materials, 4 parts of inner pattern releasing agent applicables, 135 parts of fillers, 130 parts of fibers.
Embodiment 11:
In this example, except that each proportioning raw materials had following variation, other was with embodiment 9.
Count by weight, each proportioning raw materials is: 85 parts of liquid Racemic glycidol ether type epoxies, 15 parts of solid bisphenol A type epoxy resins, 8.5 parts of thinners, 67 parts in solidifying agent, 16 parts of thickening materials, 4 parts of inner pattern releasing agent applicables, 180 parts of fillers, 150 parts of fibers.
Embodiment 12:
In this example, except that each proportioning raw materials had following variation, other was with embodiment 9.
Count by weight, each proportioning raw materials is: 75 parts of liquid Racemic glycidol ether type epoxies, 25 parts of solid bisphenol A type epoxy resins, 7.5 parts of thinners, 73 parts in solidifying agent, 12.5 parts of thickening materials, 2.5 parts of inner pattern releasing agent applicables, 130 parts of fillers, 110 parts of fibers.
Claims (9)
1. a method for preparing molded epoxy resin sheet is characterized in that adopting the binary isocyanate compound to the thickening of blending epoxy system, and chopped strand strengthens, and overlay film is prepared into the tack-free molded epoxy resin sheet of shearing,
Count by weight, this molded epoxy resin sheet is made by following raw material: 100 parts of blending epoxies, 4～10 parts of thinners, 15～80 parts in solidifying agent, 5～20 parts of thickening materials, 1～4 part of inner pattern releasing agent applicable, 80～180 parts of fillers, 50～150 parts of fibers; Wherein, blending epoxy is made up of for 10～40 parts 60～90 parts of liquid Racemic glycidol ether type epoxies and solid bisphenol A type epoxy resin; Described thickening material is 4,4 '-diphenylmethanediisocyanate, tolylene diisocyanate, 1,4-cyclohexyl diisocyanate, 2, in the 4-dimethylene diisocyanate more than one,
The preparation of this molded epoxy resin sheet specifically is to adopt the method that may further comprise the steps:
(1) preparation of epoxy paste: liquid Racemic glycidol ether type epoxy and solid bisphenol A type epoxy resin are joined in the mixing tank of band heating and heat-insulating device, and heating makes its thorough mixing; Treat that its cooling back joins in the mixing tank in proportion successively by the order of thinner, inner pattern releasing agent applicable, filler, add solidifying agent, thickening material after mixing again, mix and make epoxy paste,
(2) preparation of molded epoxy resin sheet:, epoxy paste evenly is coated on the upper and lower PE film by scraper; By the adjusting cutting unit, cutting fibre, the length of controlling fiber and content, overlay film is about to upper and lower PE film and pastes relatively then, forms the epoxy paste sheet material that a kind of above and below at fiber all is covered with the PE film; Again the epoxy paste sheet material is extruded by roller, its fiber and resin is fully flooded, be shaped to sheet material, carry out rolling then,
(3) slaking of molded epoxy resin sheet: the sheet material of rolling is transported to the thickening of thickening chamber, and the control thickening temperature is 30-60 ℃, and the sheet material thickening time is 24-240 hour, obtains described molded epoxy resin sheet.
2. the method for preparing molded epoxy resin sheet according to claim 1, it is characterized in that described liquid Racemic glycidol ether type epoxy is is that raw material prepares through polycondensation by polyphenol or polyvalent alcohol and epoxy chloropropane, it be in bisphenol A diglycidyl ether, Bisphenol F diglycidylether, the bisphenol-S diglycidyl ether more than one.
3. the method for preparing molded epoxy resin sheet according to claim 1, it is characterized in that described solid bisphenol A type epoxy resin be molecular weight greater than 900, be solid-state middle and high molecular weight bisphenol A type epoxy resin under the normal temperature.
4. the method for preparing molded epoxy resin sheet according to claim 1, it is characterized in that described thinner be in mono-epoxy compounds thinner, the multi-epoxy compounds thinner more than one.
5. the method for preparing molded epoxy resin sheet according to claim 1, it is characterized in that described solidifying agent be in aromatic amine, anhydrides, Dyhard RU 100 class, organic hydrazides class, the linear phenolic resin more than one.
6. the method for preparing molded epoxy resin sheet according to claim 1, it is characterized in that inner pattern releasing agent applicable be in stearic acid, Zinic stearas, calcium stearate, the Magnesium Stearate more than one.
7. the method for preparing molded epoxy resin sheet according to claim 1, it is characterized in that described filler be in light calcium carbonate, water-ground limestone, aluminium hydroxide, aluminum oxide, kaolin, magnesiumcarbonate, Calucium Silicate powder, silicon-dioxide, the mica more than one.
8. the method for preparing molded epoxy resin sheet according to claim 1, it is characterized in that fiber be in glass fibre, carbon fiber, the aramid fiber more than one, its length is 25-60mm.
9. molded epoxy resin sheet is characterized in that: core is by having flooded the fibrous of epoxy paste in the middle of it, and upper and lower surface covers with the PE film; Count by weight, this molded epoxy resin sheet is made by following raw material: 100 parts of blending epoxies, 4～10 parts of thinners, 15～80 parts in solidifying agent, 5～20 parts of thickening materials, 1～4 part of inner pattern releasing agent applicable, 80～180 parts of fillers, 50～150 parts of fibers; Wherein, described blending epoxy is made up of for 10～40 parts 60～90 parts of liquid Racemic glycidol ether type epoxies and solid bisphenol A type epoxy resin; Described thickening material is 4,4 '-diphenylmethanediisocyanate, tolylene diisocyanate, 1,4-cyclohexyl diisocyanate, 2, in the 4-dimethylene diisocyanate more than one.
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| CNB2007100526835A CN100564448C (en) | 2007-07-10 | 2007-07-10 | A kind of method for preparing molded epoxy resin sheet and products thereof |
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| CNB2007100526835A CN100564448C (en) | 2007-07-10 | 2007-07-10 | A kind of method for preparing molded epoxy resin sheet and products thereof |
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| CN115449187A (en) * | 2022-10-21 | 2022-12-09 | 泰州高意诚复合材料有限公司 | High-gloss and low-density SMC (sheet molding compound) material suitable for large cavity depth |
| CN115536983A (en) * | 2022-10-28 | 2022-12-30 | 泰州高意诚复合材料有限公司 | SMC (sheet molding compound) material with low glass fiber content and high rigidity |
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