CN110467791B - Unsaturated resin-based composite material and preparation method and application thereof - Google Patents
Unsaturated resin-based composite material and preparation method and application thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/01—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to unsaturated polyesters
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/08—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K2201/00—Specific properties of additives
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- C—CHEMISTRY; METALLURGY
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention relates to the field of unsaturated resin materials, in particular to an unsaturated resin-based composite material and a preparation method and application thereof. The raw materials of the unsaturated resin-based composite material comprise unsaturated resin, heat-conducting filler and a modifier, wherein the unsaturated resin is unsaturated polyester resin and/or vinyl ester resin, the heat-conducting filler is alumina and silicon carbide, the modifier is polyethylene and/or polytetrafluoroethylene, and the weight ratio of the modifier to the heat-conducting filler is (15-25): 400 to 650. The heat conductivity coefficient of the unsaturated resin-based composite material is more than 2W/m "K, which is more than 2 times of that of the traditional unsaturated polyester resin and/or vinyl ester resin-based composite material; and the unsaturated resin (unsaturated polyester resin and/or vinyl ester resin) and the heat-conducting filler have good compatibility, so that the problem of overhigh hardness caused by adding the heat-conducting filler is avoided, the Babbitt hardness of the material is less than or equal to 70, and the abrasion to a die and a contact part is reduced.
Description
Technical Field
The invention relates to the field of unsaturated resin materials, in particular to an unsaturated resin-based composite material and a preparation method and application thereof.
Background
The unsaturated resin refers to a resin containing unsaturated double bonds in the molecular chain, such as unsaturated polyester resin, vinyl ester resin, etc. The unsaturated polyester resin is one of the most commonly used thermosetting resins, and is generally a linear high molecular compound having an ester bond and an unsaturated double bond, which is obtained by polycondensation of unsaturated dibasic acid dihydric alcohol or saturated dibasic acid unsaturated dihydric alcohol. The product has good heat resistance, mechanical property, chemical corrosion resistance and dielectric property, and has wide application due to multiple varieties and low price. The vinyl ester resin not only retains the basic chain segment of the epoxy resin and has the excellent characteristics of the epoxy resin, but also introduces unsaturated double bonds into the molecular chain and has the good technological properties of the unsaturated polyester resin. Therefore, the vinyl ester resin has excellent performances in the aspects of mechanical property, high temperature resistance, chemical corrosion resistance, curing property, forming property and processing property, and is widely applied to the fields of automobiles, sports, medical treatment and health care and the like. The curing mechanism of the vinyl ester resin is the same as that of unsaturated polyester resin, the vinyl ester resin is formed by crosslinking double bonds in resin molecules and double bonds of diluent styrene, the curing time is short, the forming period is short, and the requirements of mass production of products such as composite automobile parts and the like can be met.
Although the two unsaturated resins have excellent electrical and mechanical properties, the materials have poor heat conductivity due to the application of more resins and glass fibers, and the development space of the materials is limited by the poor heat conductivity. Particularly in the field of motor plastic package, the heat dissipation problem of the high-power motor can be solved only by using a resin material with high heat conductivity coefficient, and the service life of an electric appliance is further prolonged. Thus, there is a need for improved thermal conductivity properties of unsaturated polyester/vinyl ester resins.
Conventional resin-based composites typically incorporate only aluminum hydroxide and calcium carbonate as fillers, both of which are also poor conductors of heat. By replacing part of the inorganic filler with the filler with high heat conductivity coefficient, the physical effect of improving the heat conductivity coefficient of the finished product can be achieved. For example, CN105061999A discloses several high thermal conductive fillers suitable for epoxy resin systems, specifically inorganic materials such as aluminum nitride and silicon carbide.
Although the heat conductivity coefficient of the aluminum nitride and the boron nitride is high, the water resistance of the aluminum nitride is poor, and the water resistance of a finished product is influenced; boron nitride has anisotropy, which makes the direction of heat conduction limited. The price of the aluminum hydroxide and the calcium carbonate is far higher than that of common fillers such as aluminum hydroxide and calcium carbonate, and the aluminum hydroxide and the calcium carbonate are used as main raw materials with the addition amount of more than half of the total weight, so that the market popularization of finished products is greatly limited.
Meanwhile, because the filler with high thermal conductivity has general compatibility with unsaturated polyester resin/vinyl ester resin, the filler is easily exposed during processing; the problem of too high hardness of the heat-conducting filler with moderate physical property and price exists, so that the abrasion of the heat-conducting filler to a mold in the material forming process can be greatly aggravated, and when the heat-conducting filler is applied, the abrasion of a contact part can be caused due to too high surface hardness of the material, and the production cost of a client is improved in a phase-changing manner.
Disclosure of Invention
In order to solve the technical problems, the invention provides an unsaturated resin-based composite material with high heat conductivity coefficient and moderate surface hardness, and a preparation method and application thereof.
The invention firstly provides an unsaturated resin-based composite material, which comprises raw materials of unsaturated resin, heat-conducting filler and modifier, wherein the unsaturated resin is unsaturated polyester resin and/or vinyl ester resin, the heat-conducting filler is alumina and silicon carbide, the modifier is polyethylene and/or polytetrafluoroethylene, and the weight ratio of the modifier to the heat-conducting filler is 15-25: 400 to 650.
The invention discovers that in the application environment of unsaturated polyester resin and/or vinyl ester resin, after polyethylene and/or polytetrafluoroethylene are added according to the proportion, the compatibility problem between the unsaturated resin (unsaturated polyester resin and/or vinyl ester resin) and the heat-conducting filler (alumina and silicon carbide) can be improved, and the abrasion frequency of the exposed filler to a mould can be reduced; meanwhile, the surface hardness of the molded matrix resin is reduced, and the abrasion of the matrix resin to a contact part in application is reduced or even avoided.
In order to improve the uniformity and compatibility problems when the heat-conducting filler is mixed with the unsaturated resin material and/or the vinyl ester resin and further facilitate the heat-conducting property and the surface hardness of the heat-conducting filler, the components and the using amount of the heat-conducting filler are optimized, and the following preferred scheme is obtained:
preferably, the weight ratio of the heat-conducting filler to the unsaturated resin is 400-650: 120 to 150.
In consideration of physical properties thereof, it is further preferable that the weight ratio of the alumina to the unsaturated resin is 100 to 550: 120-150, wherein the weight ratio of the silicon carbide to the unsaturated resin is 100-350: 120 to 150.
More preferably, in the above dosage range, the weight ratio of the alumina to the silicon carbide is 0.3-3: 1; more preferably 0.3 to 1: 1.
In order to improve the hardness of the material and not affect the performance of the unsaturated resin, the weight ratio of the modifier to the unsaturated resin is preferably 15-25: 120 to 150.
More preferably, the median particle diameter (D50) of the alumina is 8 to 12 μm (more preferably 10 μm); and/or the silicon carbide has a median particle diameter (D50) of 80 to 100 [ mu ] m (more preferably 90 [ mu ] m).
The invention has particularly good effect when being applied to the preparation of the bulk molding compound. Therefore, the unsaturated resin-based composite material described in the present invention is preferably a dough molding material.
In the unsaturated resin material of the present invention, the kind of the unsaturated polyester resin may be a molding material general-purpose polyester prepared by polycondensation of an unsaturated polybasic acid, a saturated polybasic acid and a polyhydric alcohol. In consideration of the working environment in actual use and the effect of compounding with the heat-conducting filler and the modifier, the unsaturated polyester resin is preferably one or a combination of more of m-benzene unsaturated polyester, o-benzene unsaturated polyester and halogenated unsaturated polyester.
Wherein, the m-benzene unsaturated polyester adopts m-phthalic acid as saturated polybasic acid, and has good mechanical property after molding; the phthalic acid is used as saturated polybasic acid in the phthalic unsaturated polyester, so that the cost is relatively low and the application is wide; the halogenated unsaturated polyester adopts halogenated saturated acid as saturated polybasic acid, so that the flame retardant grade of the product can be effectively improved.
In addition, besides the unsaturated polyester material, vinyl ester resin can be added, and the vinyl ester resin is synthesized by epoxy resin and unsaturated monoacid, and modified raw materials such as bisphenol A are introduced, so that the product can have good toughness, heat resistance and corrosion resistance.
The unsaturated resin material can be selected and compounded by persons in the field according to different requirements on the toughness, heat resistance, flame retardance, corrosion resistance and other properties of the material, and is not further limited herein.
The raw materials of the present invention may also be provided with a flame retardant filler, which is preferably aluminum hydroxide in order to achieve the properties of the unsaturated polyester resin and/or vinyl ester resin per se, corresponding to the flame retardant requirements required by some environments.
Preferably, the flame-retardant filler is used in an amount of 0 to 30 wt% based on the total weight of the composite material; preferably, the total amount of the flame-retardant filler and the heat-conducting filler is 60-70 wt%.
The amount of the flame-retardant filler and the amount of the heat-conducting filler can be adjusted according to different requirements of different customers on heat conduction, flame retardance and molding.
In some embodiments, the raw materials of the unsaturated resin-based composite material further comprise a low shrinkage agent, preferably polystyrene, in view of compatibility problems in the system of the present invention.
Meanwhile, the polyethylene and the polytetrafluoroethylene can also have the effect of a low shrinking agent, so that the dosage of the low shrinking agent in the formula can be reduced. Preferably, the low shrinkage agent is used in an amount of 1.5-2.5 wt% based on the total weight of the composite material; preferably, the total amount of the low shrinkage agent and the modifier is 3.5-4.5 wt%.
Preferably, the raw materials of the unsaturated resin-based composite material further comprise reinforcing fibers, and the reinforcing fibers are preferably chopped glass fibers.
The chopped glass fiber of the invention is used as the main body of the reinforcing material without special requirements, and can be used as long as the chopped glass fiber can be uniformly infiltrated and dispersed in an unsaturated polyester resin and/or vinyl ester resin system after surface treatment. The chopped glass fiber with the length of 1.5-12 mm can be adopted according to the actual size and strength requirements of the actual product, and under the length range, the chopped glass fiber can be selected from one or a combination of more than one of 1.5mm, 3mm, 6mm, 9mm and 12 mm;
preferably, the reinforcing fiber is used in an amount of 10 to 15 wt% based on the total weight of the composite material.
In some technical schemes, the raw materials of the unsaturated resin-based composite material also comprise one or more of a curing agent, a cross-linking agent and a release agent, and the invention further researches the preferable components when the functional agent is applied to obtain the following technical scheme:
the curing agent in the invention is organic peroxide, and specifically can adopt one or a combination of more of tert-butyl peroxybenzoate, tert-butyl peroxyisooctanoate, dibenzoyl peroxide and dicumyl peroxide.
The cross-linking agent is a free radical polymerization unsaturated monomer, has the functions of bridging the main chain of unsaturated polyester resin and/or vinyl ester resin in the forming process to solidify the unsaturated polyester resin and/or vinyl ester resin, and simultaneously has a certain dilution effect on the resin before forming, and the small molecular monomer is volatile, so that the flammability of the unsaturated resin matrix composite material before forming is improved, and the dosage is moderate. Specifically, one or a combination of more of styrene, diallyl phthalate and methyl methacrylate may be used.
The release agent is preferably one or more of stearic acid, zinc stearate, calcium stearate, aluminum stearate and magnesium stearate.
Based on the total weight of the composite material, the amount of the curing agent is 0.1-0.5 wt%; the dosage of the cross-linking agent is 1.5-2.5 wt%; the using amount of the release agent is 1.5-2.5 wt%.
As a preferred technical scheme, the invention provides an unsaturated resin-based composite material (bulk molding compound), which comprises the following raw materials:
the above-described preferred embodiments can be combined by one skilled in the art to provide preferred embodiments of the present invention.
The invention further provides a preparation method of the unsaturated resin-based composite material, which comprises the steps of mixing organic raw materials including the unsaturated resin and the modifier to obtain a first premix (preferably mixing for 2-5 min), mixing the first premix with inorganic raw materials including the heat-conducting filler to obtain a second premix (preferably mixing for 25-30 min), and finally mixing the second premix with the reinforcing fibers.
During the preparation process, special attention needs to be paid to slowly adding the reinforcing fiber into a kneader so as to avoid uneven mixing. The kneading time cannot be too long so as to avoid fiber damage and cause great reduction of product strength. In the present invention, the mixing time with the reinforcing fiber is preferably 6 to 8 min.
The invention further provides the application of the unsaturated resin-based composite material or the unsaturated resin-based composite material prepared by the preparation method in medium and small-sized circuit breakers, electrical insulators, automobile large lamp reflectors and plastic package motors; preferably applied to plastic package motors.
The invention has the following beneficial effects:
the heat conductivity coefficient of the unsaturated resin-based composite material is more than 2W/m "K, which is more than 2 times of that of the traditional unsaturated polyester resin and/or vinyl ester resin-based composite material; and the unsaturated resin (unsaturated polyester resin and/or vinyl ester resin) and the heat-conducting filler have good compatibility, so that the problem of overhigh hardness caused by adding the heat-conducting filler is avoided, the Babbitt hardness of the material is less than or equal to 70, and the abrasion to a die and a contact part is reduced. In addition, the stability of the material is improved and the product quality is improved by improving the compatibility among the components.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In order to illustrate the effects by comparison, the invention is verified by using bulk molding compounds of different formulations and the effects of the implementation thereof, the formulations of the examples and the comparative examples are as shown in table 1 below, and in the following examples, the amounts of the components are mass amounts.
TABLE 1
The preparation of each bulk molding compound in the above table is as follows:
and (2) adding unsaturated polyester resin, a cross-linking agent, a curing agent, a low shrinkage agent, a modifier (showing "-" in a table is not added) and a release agent into a double-arm kneader in sequence, then reversely rotating the paddle for 2-5 min, then adding a heat-conducting filler and/or a flame-retardant filler (showing "-" in the table is not added) according to the formula, positively rotating the paddle for 25-30 min, finally adding a reinforcing fiber, and obtaining the bulk molding compound with high heat conductivity coefficient after 6-8 min.
The effects of the bulk molding compounds of the examples and comparative examples are shown in Table 2 below.
TABLE 2
All the sample strips on the upper table are molded by using 140 ℃/10MPa, and the curing time of the sample strips in different items is adjusted according to the thickness of the sample strips, wherein the standard is 60 sec/mm;
the Babbitt hardness was measured using a Babbitt hardness meter HBa-1 developed by the commercial Measure science research institute of Sn-free;
the thermal conductivity (hot wire method) was measured using a Kyoto Electronic (KEM) QTM-500 model fast hot wire method thermal conductivity meter.
From the above data, the embodiments of the formulation of the present invention can reduce the hardness of the surface of the material while having a higher thermal conductivity.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (14)
1. The unsaturated resin-based composite material comprises unsaturated resin and heat-conducting filler, and is characterized in that the raw material further comprises a modifier, the unsaturated resin is unsaturated polyester resin and/or vinyl ester resin, the heat-conducting filler is aluminum oxide and silicon carbide, the modifier is polyethylene and/or polytetrafluoroethylene, and the weight ratio of the modifier to the heat-conducting filler is 15-25: 400-650;
the weight ratio of the heat-conducting filler to the unsaturated resin is 400-650: 120 to 150.
2. The unsaturated resin-based composite material according to claim 1, wherein the weight ratio of the alumina to the unsaturated resin is 100-550: 120-150, wherein the weight ratio of the silicon carbide to the unsaturated resin is 100-350: 120 to 150 parts;
and/or the weight ratio of the aluminum oxide to the silicon carbide is 0.3-3: 1.
3. The unsaturated resin-based composite material according to claim 1, wherein the weight ratio of the modifier to the unsaturated resin is 15-25: 120 to 150.
4. The unsaturated resin-based composite material according to claim 3, wherein the median particle size of the alumina is 8-12 μm; and/or the median particle size of the silicon carbide is 80-100 mu m.
5. The unsaturated resin-based composite material according to claim 1, characterized in that the unsaturated resin-based composite material is a dough moulding plastic.
6. The unsaturated resin-based composite material according to claim 5, characterized in that the unsaturated polyester resin is one or more combinations of m-benzene type unsaturated polyester, o-benzene type unsaturated polyester, halogenated unsaturated polyester.
7. The unsaturated resin-based composite material according to claim 2, wherein the raw materials further comprise 0-30 wt% of a flame-retardant filler, the total amount of the flame-retardant filler and the heat-conducting filler is 60-70 wt%, and the flame-retardant filler is aluminum hydroxide.
8. The unsaturated resin-based composite material according to claim 3, wherein the raw materials further comprise 1.5-2.5 wt% of a low shrinkage agent, the total amount of the low shrinkage agent and the modifier is 3.5-4.5 wt%, and the low shrinkage agent is polystyrene.
9. The unsaturated resin-based composite material according to claim 1, wherein the raw materials further comprise 10-15 wt% of reinforcing fibers, and the reinforcing fibers are chopped glass fibers.
10. The unsaturated resin-based composite material according to claim 1, wherein the raw materials further comprise one or more of a curing agent, a cross-linking agent, and a release agent;
the curing agent is one or a combination of more of tert-butyl peroxybenzoate, tert-butyl peroxyisooctanoate, dibenzoyl peroxide and dicumyl peroxide;
the cross-linking agent is one or the combination of more of styrene, diallyl phthalate and methyl methacrylate;
the release agent is one or a combination of stearic acid, zinc stearate, calcium stearate, aluminum stearate and magnesium stearate.
11. The unsaturated resin-based composite material according to claim 1, characterized by comprising the following raw materials in parts by weight:
12. the method for preparing the unsaturated resin-based composite material according to any one of claims 1 to 11, wherein organic raw materials including the unsaturated resin and the modifier are mixed to obtain a first premix, the first premix is mixed with inorganic raw materials including the heat-conducting filler to obtain a second premix, and finally the second premix is mixed with the reinforcing fiber.
13. The method of claim 12, wherein the second premix is mixed with the reinforcing fiber for 6 to 8 min.
14. Use of the unsaturated resin-based composite material according to any one of claims 1 to 11 or the unsaturated resin-based composite material prepared by the preparation method according to claim 12 or 13 in medium and small-sized circuit breakers, electrical insulators, reflectors of large lamps of automobiles and plastic package motors.
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| CN104371237A (en) * | 2014-12-05 | 2015-02-25 | 上海昭和高分子有限公司 | Unsaturated polyester resin composition thickened by non-alkali metal systems and bulk molding compound with unsaturated polyester resin composition |
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