CN110467791A - A kind of unsaturated-resin based composites and the preparation method and application thereof - Google Patents
A kind of unsaturated-resin based composites and the preparation method and application thereof Download PDFInfo
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- CN110467791A CN110467791A CN201910911066.9A CN201910911066A CN110467791A CN 110467791 A CN110467791 A CN 110467791A CN 201910911066 A CN201910911066 A CN 201910911066A CN 110467791 A CN110467791 A CN 110467791A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- Macromonomer-Based Addition Polymer (AREA)
Abstract
The present invention relates to unsaturated-resin Material Fields, and in particular to a kind of unsaturated-resin based composites and the preparation method and application thereof.The raw material of the unsaturated-resin based composites includes unsaturated-resin, heat filling, and modifying agent, the unsaturated-resin is unsaturated polyester resin and/or vinyl ester resin, the heat filling is aluminium oxide and silicon carbide, the modifying agent is polyethylene and/or polytetrafluoroethylene (PTFE), and the weight ratio of the modifying agent and the heat filling is 15~25:400~650.The thermal coefficient > 2W/m 〃 K of unsaturated-resin based composites, is the 2 times or more of traditional unsaturated polyester resin and/or vinyl ester resin based composites in the present invention；And there is good compatibility between unsaturated-resin (unsaturated polyester resin and/or vinyl ester resin) and heat filling, avoid because be added heat filling and caused by excessive high hardness the problem of, hardness Barcol≤70 of material reduce the abrasion to mold and contact component.
Description
Technical field
The present invention relates to unsaturated-resin Material Fields, and in particular to a kind of unsaturated-resin based composites and its preparation
Method and application.
Background technique
Unsaturated-resin refers to the resin in strand containing unsaturated double-bond, such as unsaturated polyester resin, vinyl esters tree
Rouge etc..Unsaturated polyester resin is most common one kind in thermosetting resin, usually by unsaturated dibasic acid dihydric alcohol or
With the chain macromolecule compound of ester bond and unsaturated double-bond made of monounsaturated dicarboxylic acid unsaturation dihydric alcohol polycondensation.Due to it
With preferable heat resistance, mechanical property, resistance to chemical corrosion and dielectric properties, and it is wide in variety, price is lower, therefore by
Extensive use is arrived.Vinyl ester resin had both remained the basic segment of epoxy resin, had adhered to the good characteristic of epoxy resin,
Unsaturated double-bond is introduced in strand again, the good process performance with unsaturated polyester resin.So vinyl esters tree
Rouge has in terms of mechanical property, high temperature resistance, resistance to chemical corrosion and curing performance, processability and processing performance
Outstanding performance is all widely used in fields such as automobile, sport, health cares.The curing of vinyl ester resin
Reason is identical as unsaturated polyester resin, is the cross moulding between the double bond in molecular resin and the double bond of diluent styrene, Gu
The change time is short, short molding cycle, can satisfy the demand of the product batches such as composite material automobile parts production.
Although two kinds of above-mentioned unsaturated-resins are in electric property, mechanical performance etc. is excellent in, due to wherein
It is the non-conductor of heat using more resin and glass, therefore the heating conduction of material is bad, and it is this thermally conductive undesirable
Characteristic increasingly constrains the space of its development.Especially in motor plastic packaging field, only has the resinous wood of high thermal conductivity coefficient
Material just can solve the heat dissipation problem of high power motor, and then extend the service life of electric appliance.Therefore, it needs to unsaturated polyester (UP) tree
Rouge/vinyl ester resin heating conduction improves.
Aluminium hydroxide and calcium carbonate is usually only added as filler in traditional polymer matrix composites, and the two is also all
The non-conductor of heat.By the way that part inorganic filler to be replaced with to the filler of high thermal conductivity coefficient, it can play and improve the thermally conductive system of finished product
Several physical effects.Such as CN105061999A discloses several high thermal conductivity fillers suitable for epoxy-resin systems, specially
The inorganic material such as aluminium nitride and silicon carbide.
Although the thermal coefficient of aluminium nitride and boron nitride itself is high, the poor water resistance of aluminium nitride will affect the resistance to of finished product
Aqueous energy；Boron nitride has anisotropy, and thermally conductive direction can be made limited.And the price of said two devices is all significantly larger than hydroxide
The customary fillers such as aluminium and calcium carbonate, are more than the primary raw material of gross weight half as additive amount, this will greatly limit the city of finished product
It promotes field.
Simultaneously as such filler for having high thermal conductivity coefficient is compatible with unsaturated polyester resin/vinyl ester resin
Property it is general, processing when be easy to happen the exposed situation of filler；And physical property and moderate heat filling itself there is
The problem of excessive high hardness, leads to it not only and can substantially aggravate the abrasion in material forming process to mold, in use, also can be because
For material surface excessive high hardness, the abrasion to contact component is caused, in a disguised form improves the production cost of client.
Summary of the invention
It is high that in order to solve the above-mentioned technical problems, the present invention provides a kind of thermal coefficients, the moderate unsaturation of surface hardness
Polymer matrix composites and the preparation method and application thereof.
Present invention firstly provides a kind of unsaturated-resin based composites, raw material includes unsaturated-resin, heat filling,
And modifying agent, the unsaturated-resin are unsaturated polyester resin and/or vinyl ester resin, the heat filling is oxidation
Aluminium and silicon carbide, the modifying agent are polyethylene and/or polytetrafluoroethylene (PTFE), the weight ratio of the modifying agent and the heat filling
For 15~25:400~650.
It is a discovery of the invention that in the application environment of unsaturated polyester resin and/or vinyl ester resin, according to the above ratio plus
After entering polyethylene and/or polytetrafluoroethylene (PTFE), unsaturated-resin (unsaturated polyester resin and/or vinyl ester resin) can be improved
With the consistency problem between heat filling (aluminium oxide and silicon carbide), the exposed abrasion frequency to mold of filler is reduced；Simultaneously
Matrix resin surface hardness after molding is reduced, reduces and even avoids its abrasion in application to contact component.
In order to improve homogeneity when heat filling is mixed with unsaturated-resin material and/or vinyl ester resin and compatible
Property problem, is further conducive to take into account its heating conduction and surface hardness, the present invention carries out heat filling component and dosage
Optimization, obtains following preferred embodiment:
Preferably, the weight ratio of the heat filling and the unsaturated-resin is 400~650:120~150.
Take the physical property of itself into consideration, the weight ratio of the further preferred aluminium oxide and the unsaturated-resin
For 100~550:120~150, the weight ratio of the silicon carbide and the unsaturated-resin is 100~350:120~150.
More preferably in above-mentioned amount ranges, the weight ratio of the aluminium oxide and silicon carbide is 0.3~3:1；It is further excellent
It is selected as 0.3~1:1.
It is preferably described to change in order to while improving material hardness, not influence performance possessed by unsaturated-resin itself
Property agent and the unsaturated-resin weight ratio be 15~25:120~150.
It is further preferred that the median (D50) of the aluminium oxide is 8~12 μm (more preferably 10 μm)；And/or
The median (D50) of the silicon carbide is 80~100 μm (more preferably 90 μm).
For the present invention when being applied to group's die-filling plastics preparation, it is especially good to have the effect of.It is therefore preferable that heretofore described
Unsaturated-resin based composites be the die-filling plastics of group.
In unsaturated-resin material of the invention, the type of unsaturated polyester resin can be by unsaturated polyacid,
Moulding material general purpose polyester made of saturated polybasic acid and polyhydric alcohol.In view of working environment in actual use, and
The effect compounded with the heat filling, modifying agent, the preferably described unsaturated polyester resin are metaphenylene unsaturated polyester (UP), adjacent benzene
One of type unsaturated polyester (UP), halogenated unsaturated polyester (UP) or multiple combinations.
Wherein, metaphenylene unsaturated polyester (UP) uses M-phthalic acid as saturated polybasic acid, has after molding good
Mechanical property；Adjacent benzene-type unsaturated polyester (UP) uses phthalic acid as saturated polybasic acid, and advantage of lower cost is widely used；
Halogenated unsaturated polyester (UP), as saturated polybasic acid, can effectively promote the flame retardant rating of product using halogenated saturated acid.
In addition, vinyl ester resin, the vinyl ester resin can also be added in addition to above-mentioned unsaturated polyester material
Synthesize by epoxy resin with unsaturated monoacid, after the modified feedstocks such as introducing bisphenol-A, can assign the good toughness of product,
Heat resistance and corrosion resistance.
Those skilled in the art can according to the different demands of the performances such as toughness, heat resistance, anti-flammability, corrosion resistance to material,
Above-mentioned unsaturated-resin material is selected and compounded, is not further limited herein.
Fire-retardant filler can also be arranged in flame-retardancy requirements needed for corresponding part environment, raw material of the invention, in order to balance not
The performance of saturated polyester resin and/or vinyl ester resin itself, the fire-retardant filler are preferably aluminium hydroxide.
Preferably, the dosage of the fire-retardant filler is 0~30wt% on the basis of composite material gross weight；It is preferred that described
Total dosage of fire-retardant filler and the heat filling is 60~70wt%.
It, can be to the use of fire-retardant filler and heat filling according to different clients to thermally conductive, fire-retardant and molding different requirements
Amount is adjusted.
Further include shrinking agent in the raw material of the unsaturated-resin based composites in some technical solutions, considers
To consistency problem in the present invention system, the shrinking agent is preferably polystyrene.
Simultaneously as polyethylene, polytetrafluoroethylene (PTFE) itself can also have the function of shrinking agent, therefore can also reduce
The dosage of shrinking agent in prescription.It is preferred that on the basis of composite material gross weight, the dosage of the shrinking agent is 1.5~
2.5wt%；It is preferred that total dosage of the shrinking agent and the modifying agent is 3.5~4.5wt%.
Preferably, further include reinforcing fiber in the raw material of the unsaturated-resin based composites, the reinforcing fiber
Preferably short glass fiber.
Short glass fiber in the present invention does not have particular/special requirement as reinforcing material main body, as long as at by surface
Reason, can the kind that is dispersed in unsaturated polyester resin and/or vinyl ester resin systems of homogeneous immersion can be used.It can basis
The actual size and intensity requirement of actual product use length for the short glass fiber of 1.5~12mm, under the length range,
Short glass fiber can select one of 1.5mm, 3mm, 6mm, 9mm, 12mm or multiple combinations；
It is preferred that the dosage of the reinforcing fiber is 10~15wt% on the basis of composite material gross weight.
In some technical solutions, further include in the raw material of the unsaturated-resin based composites curing agent, crosslinking agent,
One or more of release agent, the present invention further to application above-mentioned functional agent when preferred ingredient study, obtain as
Lower technical solution:
Curing agent in the present invention is organic peroxide, and it is different that peroxidized t-butyl perbenzoate, peroxidating specifically can be used
One of octanoic acid ter-butyl ester, dibenzoyl peroxide, cumyl peroxide or multiple combinations.
Crosslinking agent in the present invention is free-radical polymerised unsaturated monomer, and effect is that unsaturation is bridged in forming process
Polyester resin and/or vinyl ester resin main chain are allowed to solidify, while also can generate certain diluting effect to resin before forming,
And small molecule monomer is volatile, the inflammability before improving the unsaturated-resin based composites molding, therefore used in amounts is moderate.
One of styrene, diallyl phthalate ester and methyl methacrylate or multiple combinations specifically can be used.
The release agent be preferably one of stearic acid, zinc stearate, calcium stearate, aluminum stearate, magnesium stearate or
Multiple combinations.
On the basis of composite material gross weight, the dosage of the curing agent is 0.1~0.5wt%；The dosage of the crosslinking agent
For 1.5~2.5wt%；The dosage of the release agent is 1.5~2.5wt%.
As a kind of perferred technical scheme, the present invention provides a kind of unsaturated-resin based composites (bulk molding
Material), including the following raw material:
Those skilled in the art can be combined above-mentioned preferred embodiment, obtain present pre-ferred embodiments.
The present invention further provides the preparation methods of the unsaturated-resin based composites, first will include the insatiable hunger
It is mixed to get the first premix (preferably mixing 2~5min) with the Organic Ingredients including resin, the modifying agent, then by described the
One premix and the inorganic raw material including the heat filling be mixed to get the second premix (preferably mix 25~
30min), finally second premix is mixed with reinforcing fiber.
In preparation process, to pay special attention to reinforcing fiber need to be slowly added into kneader, in case mixing is uneven.Kneading time
Cannot be too long, in case fibre damage, causes product strength sharp fall.In the present invention, it is preferred to mixed with reinforcing fiber
Time is 6~8min.
The present invention further provides the unsaturated-resin based composites or through insatiable hunger made from above-mentioned preparation method
With application of the polymer matrix composites in small-medium size breaker, electric equipment insulator, headlight for vehicles reflecting mirror, plastic packaging motor；
It is preferred that the application in plastic packaging motor.
The present invention has the beneficial effect that:
The thermal coefficient > 2W/m 〃 K of unsaturated-resin based composites, is traditional unsaturated polyester resin in the present invention
And/or the 2 times or more of vinyl ester resin based composites；And unsaturated-resin (unsaturated polyester resin and/or vinyl
Ester resin) and heat filling between have good compatibility, avoid because be added heat filling and caused by excessive high hardness
The problem of, hardness Barcol≤70 of material reduce the abrasion to mold and contact component.In addition, by between compatible component
The improvement of property, also improves the stability of material, improves product quality.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
In order to which by comparative illustration effect, the present invention is tested by the tubular molding compound and its implementation result of different formulations
Card, embodiment and comparative formulation such as the following table 1, in following embodiment, the dosage of each component is quality dosage.
Table 1
The preparation process of each tubular molding compound is as follows in upper table:
Unsaturated polyester resin, crosslinking agent, curing agent, shrinking agent, modifying agent are sequentially added in two-arm kneader
After (showing that "-" is just not added in table), release agent, blade invert 2~5min, then according to formula be added heat filling and/or
Fire-retardant filler (shows that "-" is just not added) in table, blade rotates forward 25~30min, is eventually adding reinforcing fiber, 6~8 minutes, i.e.,
Can must have the tubular molding compound of high thermal conductivity coefficient.
The implementation result of each tubular molding compound see the table below 2. in embodiment and comparative example
Table 2
Upper all battens of table use 140 DEG C/10MPa to be molded, and the curing time of disparity items batten is according to batten thickness
It is adjusted, standard 60sec/mm；
Hardness Barcol is developed HBa-1 Bareol hardness meter using Wuxi City metering scientific research institute and is measured；
Thermal coefficient (heat-pole method) is measured using the quick heat-pole method thermal conductivity factor instrument of capital of a country electronics (KEM) QTM-500 type.
It can be obtained by upper table data, the embodiment of inventive formulation can make material while with high thermal conductivity,
Reduce the hardness on its surface.
Although above having used general explanation, specific embodiment and test, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (15)
1. a kind of unsaturated-resin based composites, raw material include unsaturated-resin and heat filling, which is characterized in that described
Raw material further includes modifying agent, and the unsaturated-resin is unsaturated polyester resin and/or vinyl ester resin, the heat filling
For aluminium oxide and silicon carbide, the modifying agent is polyethylene and/or polytetrafluoroethylene (PTFE), the modifying agent and the heat filling
Weight ratio is 15~25:400~650.
2. unsaturated-resin based composites according to claim 1, which is characterized in that the heat filling and it is described not
The weight ratio of saturated resin is 400~650:120~150.
3. unsaturated-resin based composites according to claim 2, which is characterized in that the aluminium oxide and the insatiable hunger
It is 100~550:120~150 with the weight ratio of resin, the weight ratio of the silicon carbide and the unsaturated-resin is 100~
350:120~150；
And/or the weight ratio of the aluminium oxide and silicon carbide is 0.3~3:1.
4. unsaturated-resin based composites according to claim 1, which is characterized in that the modifying agent and the insatiable hunger
Weight ratio with resin is 15~25:120~150.
5. unsaturated-resin based composites according to claim 4, which is characterized in that the median of the aluminium oxide
It is 8~12 μm；And/or the median of the silicon carbide is 80~100 μm.
6. unsaturated-resin based composites according to claim 1, which is characterized in that the unsaturated-resin base is compound
Material is the die-filling plastics of group.
7. unsaturated-resin based composites according to claim 6, which is characterized in that the unsaturated polyester resin is
One of metaphenylene unsaturated polyester (UP), adjacent benzene-type unsaturated polyester (UP), halogenated unsaturated polyester (UP) or multiple combinations.
8. unsaturated-resin based composites according to claim 3, which is characterized in that the raw material further includes 0~
Total dosage of 30wt% fire-retardant filler, the fire-retardant filler and the heat filling is 60~70wt%, and the fire-retardant filler is
Aluminium hydroxide.
9. unsaturated-resin based composites according to claim 4, which is characterized in that the raw material further includes 1.5~
Total dosage of 2.5wt% shrinking agent, the shrinking agent and the modifying agent is 3.5~4.5wt%, and the shrinking agent is
Polystyrene.
10. unsaturated-resin based composites according to claim 1, which is characterized in that the raw material further includes 10~
15wt% reinforcing fiber, the reinforcing fiber are short glass fiber.
11. unsaturated-resin based composites according to claim 1, which is characterized in that the raw material further includes solidification
One or more of agent, crosslinking agent, release agent；
The curing agent is peroxidized t-butyl perbenzoate, the peroxidating isooctyl acid tert-butyl ester, dibenzoyl peroxide, peroxidating two
One of isopropylbenzene or multiple combinations；
The crosslinking agent is one of styrene, diallyl phthalate ester and methyl methacrylate or multiple combinations；
The release agent is one of stearic acid, zinc stearate, calcium stearate, aluminum stearate, magnesium stearate or multiple combinations.
12. unsaturated-resin based composites described according to claim 1~any one of 11, which is characterized in that including such as
The raw material of lower parts by weight:
13. the preparation method of unsaturated-resin based composites described in any one of claim 1~12, which is characterized in that
The Organic Ingredients including the unsaturated-resin, the modifying agent is first mixed to get the first premix, then by described
One premix is mixed to get the second premix with the inorganic raw material including the heat filling, finally premixes described second
Material is mixed with reinforcing fiber.
14. preparation method described in claim 13, which is characterized in that the time that second premix is mixed with reinforcing fiber
For 6~8min.
15. described in unsaturated-resin based composites or claim 13 or 14 described in any one of claim 1~12
Unsaturated-resin based composites made from preparation method small-medium size breaker, electric equipment insulator, headlight for vehicles reflecting mirror,
Application in plastic packaging motor.
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| CN201910911066.9A CN110467791B (en) | 2019-09-25 | 2019-09-25 | Unsaturated resin-based composite material and preparation method and application thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120077921A1 (en) * | 2009-06-24 | 2012-03-29 | Ryujin Ishiuchi | Unsaturated polyester resin composition and encapsulated motor |
| 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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2019
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120077921A1 (en) * | 2009-06-24 | 2012-03-29 | Ryujin Ishiuchi | Unsaturated polyester resin composition and encapsulated motor |
| 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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Address after: 8333 Songze Avenue, Qingpu Industrial Park, Qingpu District, Shanghai, 201707 Patentee after: Lisennoco Polymer Materials (Shanghai) Co.,Ltd. Address before: 8333 Songze Avenue, Qingpu Industrial Park, Qingpu District, Shanghai, 201707 Patentee before: SHANGHAI SHOWA HIGHPOLYMER CO.,LTD. |
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