CN110305446A - A kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model - Google Patents
A kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model Download PDFInfo
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- CN110305446A CN110305446A CN201910575876.1A CN201910575876A CN110305446A CN 110305446 A CN110305446 A CN 110305446A CN 201910575876 A CN201910575876 A CN 201910575876A CN 110305446 A CN110305446 A CN 110305446A
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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08K7/00—Use of ingredients characterised by shape
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention relates to epoxide resin material technical fields, specifically a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model, the raw material comprising following parts by weight of component: 100 parts of epoxy resin, 50 parts of curing agent, 20-25 parts of boron nitride, 5-10 parts of silicon carbide, 60-80 parts of conductive filler, 0.5-2 parts of silane coupling agent, 5-8 parts of heat stabilizer.The present invention provides a kind of epoxy resin for having both high temperature resistant and electric conductivity, and it is practiced in the preparation of slush mold epoxy core model, so that epoxy core model has good surface conductivity, electroforming can directly be carried out by not needing progress conductive treatment, fundamentally solve deficiency existing for traditional conductive treatment technique.
Description
Technical field
It is specifically a kind of to be applied to prepared by slush mold epoxy core model the present invention relates to epoxide resin material technical field
High temperature resistant conductive epoxy resin.
Background technique
Epoxy resin has the adaptability of rapid die-manufacturing, reliable surface replication, splendid dimensional stability and wear-resisting
Property, high temperature resistant, it is light-weight and inexpensive the advantages that, therefore be widely used in mould manufacturing field；In recent years due to epoxy
Resin die has many advantages, such as that molding speed is fast, at low cost, and epoxy resin has been widely used in automobile interior decoration slush molding side
The Mould design and manufacturing in face.In view of the preparation process of slush mold, epoxy core model made of epoxy resin needs to have centainly
High temperature resistance and good surface conductivity, therefore usually require to improve in actual production its heat resistance and to carry out surface
Conductive treatment.
108707390 A of Chinese patent CN discloses a kind of super heat resistant epoxide resin composite coating and preparation method thereof, leads to
The addition for crossing heat filling solves the problems, such as that epoxy resin heat resistance is poor to a certain extent, but active during the preparation process
The addition of diluent can affect to the cross-linking and curing reaction of epoxy resin, reduce the curing degree of epoxy resin, shadow
Ring its service performance.Chinese patent CN103737762A discloses a kind of production method of decorative pattern copy mold electroforming core model, gram
The cumbersome of existing core model manufacturing process is taken, but the patent is to propose a kind of novel production method, is not directed to technique
The selection of middle epoxy resin and conductive formula.104674202 A of Chinese patent CN discloses a kind of slush mold and enters channel mould surface
Metallizing treatment process optimizes the technique for spraying silver-colored process, solves activation process and silver ammino solution in previous conductive treatment
The environmental issue of formula；But realize the homogeneous coating of epoxy mandrel surface, requirement of this method to operator is very high, in addition exists
The caking property of coating and epoxy core model need to be considered during electroforming.107699875 A of Chinese patent CN discloses one kind and wards off
The Electroless Silver Plating of mould, the technique improve the knot between coating and matrix by adjusting the solution of roughening and sensitising step
With joint efforts, with tradition it is silver-plated operation and no significant difference；Acid processing in roughening and activation process will certainly be to epoxy core model table
The fine decorative pattern in face causes to corrode, and influences decorative pattern fidelity.
In conclusion the conductive treatment technique of slush mold epoxy core model is main or with traditional chemical silvering at present
Based on technique, it is aided with the formulation optimization of certain steps；But this can not fundamentally solve the defect of Electroless Silver Plating.
Summary of the invention
The purpose of the present invention is to provide a kind of high temperature resistant conductive epoxies applied to the preparation of slush mold epoxy core model
Rouge, to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model includes following parts by weight of component
Raw material: 100 parts of epoxy resin, 50 parts of curing agent, 20-25 parts of boron nitride, 5-10 parts of silicon carbide, 60-80 parts of conductive filler, silicon
0.5-2 parts of alkane coupling agent, 5-8 parts of heat stabilizer.
As a further solution of the present invention: the epoxy resin is bisphenol f type epoxy resin, viscosity 1000-
2000mPa·s。
As a further solution of the present invention: the curing agent is fatty amines curing agent, viscosity 150mPas.
As a further solution of the present invention: the boron nitride particles are spherical shape, and average grain diameter is 1 μm.
As a further solution of the present invention: the silicon carbide is nanometer particle, average grain diameter 100nm.
As a further solution of the present invention: the conductive filler is one or more, the pattern of metallic Ag and Cu
For sheet or spherical, and average grain diameter is 5-10 μm.
As a further solution of the present invention: the silane coupling agent is γ-aminopropyl triethoxysilane and γ-
One of (the third oxygen of 2,3- epoxy) propyl trimethoxy silicane is a variety of.
As a further solution of the present invention: the heat stabilizer is one of barium stearate and calcium-zinc composite stabilizing agent
Or it is a variety of.
As a further solution of the present invention: preparation process specifically:
(1) it weighs conductive filler, boron nitride, silicon carbide and silane coupling agent in proportion to be mixed, and in 25 DEG C of ring
It is ultrasonically treated 1h under border, obtains composite mortar；
(2) composite mortar and epoxy resin are mixed and stirred for, revolving speed 1000rpm, time 10min；
(3) then, heat stabilizer and toughener are proportionally added into and is stirred, revolving speed 500rpm, time 5min,
(4) it is finally proportionally added into curing agent, stirs and deaeration is handled, obtain mixture；
(5) mixture is brushed and is reprinted on mould in slush mold silica gel, be placed in solidification in thermostatic drying chamber, obtain high temperature resistant
Conductive epoxy core model.
As a further solution of the present invention: in the step (5), solidification temperature is 60-80 DEG C, curing time 10-
12h brushes with a thickness of 5-10mm.
Compared with prior art, the beneficial effects of the present invention are: the present invention provides one kind to have both high temperature resistant and electric conductivity
Epoxy resin, and the preparation of slush mold epoxy core model is practiced in, so that epoxy core model has good surface conductance
Property, electroforming can directly be carried out by not needing progress conductive treatment, fundamentally solved traditional conductive treatment technique and deposited
Deficiency.High temperature resistant conductive epoxy resin provided by the invention has the advantages that high temperature resistant, viscosity are low, and has excellent lead
Electrically, it finds after tested, conductivity reaches as high as 10-2S/m, meets the performance requirement (conductivity > 10-4S/m) of subsequent electroforming.
The preparation method simple process of high temperature resistant conductive epoxy resin provided by the invention, it is easy to operate.
Detailed description of the invention
Fig. 1 is conductive epoxy core mold structure schematic diagram；
Fig. 2 is the high temperature resistant conductive epoxy core model with fine textures；
Fig. 3 is gained nickel shell after electroforming；
Fig. 4 is the nickel crystalline form looks (200X) of nickel shell mold tool under an optical microscope；
Fig. 5 is the microstructure of 1 section of embodiment.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
In the description of the present invention, it is to be understood that, term " center ", " longitudinal direction ", " transverse direction ", "upper", "lower",
The orientation or positional relationship of the instructions such as "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside" is
It is based on the orientation or positional relationship shown in the drawings, is merely for convenience of description of the present invention and simplification of the description, rather than instruction or dark
Show that signified device or element must have a particular orientation, be constructed and operated in a specific orientation, therefore should not be understood as pair
Limitation of the invention.In addition, term " first ", " second " etc. are used for description purposes only, it is not understood to indicate or imply phase
To importance or implicitly indicate the quantity of indicated technical characteristic.The feature for defining " first ", " second " etc. as a result, can
To explicitly or implicitly include one or more of the features.In the description of the present invention, unless otherwise indicated, " multiple "
It is meant that two or more.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also can be indirectly connected through an intermediary
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood by concrete condition
Concrete meaning in the present invention.
The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
Embodiment one
A kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model includes following parts by weight of component
Raw material: 100 parts of epoxy resin, 50 parts of curing agent, 20 parts of boron nitride, 5 parts of silicon carbide, 60 parts of conductive filler, silane coupling agent
0.5 part, 5 parts of heat stabilizer.
The epoxy resin is bisphenol f type epoxy resin, viscosity 1000mPas, and the curing agent is solid for fatty amines
Agent, viscosity 150mPas, the boron nitride particles are spherical shape, and average grain diameter is 1 μm, and the silicon carbide is nanometer
Grade particle, average grain diameter 100nm, the conductive filler are one kind of metallic Ag and Cu, and pattern is sheet or spherical, and
Average grain diameter is 5 μm, and the silane coupling agent is γ-aminopropyl triethoxysilane and γ-(2,3- the third oxygen of epoxy) propyl
One of trimethoxy silane is a variety of, and the heat stabilizer is one of barium stearate and calcium-zinc composite stabilizing agent or more
Kind.
Preparation process specifically:
(1) it weighs conductive filler, boron nitride, silicon carbide and silane coupling agent in proportion to be mixed, and in 25 DEG C of ring
It is ultrasonically treated 1h under border, obtains composite mortar；
(2) composite mortar and epoxy resin are mixed and stirred for, revolving speed 1000rpm, time 10min；
(3) then, heat stabilizer and toughener are proportionally added into and is stirred, revolving speed 500rpm, time 5min,
(4) it is finally proportionally added into curing agent, stirs and deaeration is handled, obtain mixture；
(5) mixture is brushed and is reprinted on mould in slush mold silica gel, be placed in solidification in thermostatic drying chamber, obtain high temperature resistant
Conductive epoxy core model.
In the step (5), solidification temperature is 60 DEG C, curing time 10h, is brushed with a thickness of 5mm.
Embodiment two
A kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model includes following parts by weight of component
Raw material: 100 parts of epoxy resin, 50 parts of curing agent, 25 parts of boron nitride, 10 parts of silicon carbide, 80 parts of conductive filler, silane coupling agent
2 parts, 8 parts of heat stabilizer.
The epoxy resin is bisphenol f type epoxy resin, viscosity 2000mPas, and the curing agent is solid for fatty amines
Agent, viscosity 150mPas, the boron nitride particles are spherical shape, and average grain diameter is 1 μm, and the silicon carbide is nanometer
Grade particle, average grain diameter 100nm, the conductive filler are the mixing of metallic Ag and Cu, and pattern is sheet or spherical, and
Average grain diameter is 10 μm, and the silane coupling agent is γ-aminopropyl triethoxysilane and γ-(2,3- the third oxygen of epoxy) propyl
One of trimethoxy silane is a variety of, and the heat stabilizer is one of barium stearate and calcium-zinc composite stabilizing agent or more
Kind.
Preparation process specifically:
(1) it weighs conductive filler, boron nitride, silicon carbide and silane coupling agent in proportion to be mixed, and in 25 DEG C of ring
It is ultrasonically treated 1h under border, obtains composite mortar；
(2) composite mortar and epoxy resin are mixed and stirred for, revolving speed 1000rpm, time 10min；
(3) then, heat stabilizer and toughener are proportionally added into and is stirred, revolving speed 500rpm, time 5min,
(4) it is finally proportionally added into curing agent, stirs and deaeration is handled, obtain mixture；
(5) mixture is brushed and is reprinted on mould in slush mold silica gel, be placed in solidification in thermostatic drying chamber, obtain high temperature resistant
Conductive epoxy core model.
In the step (5), solidification temperature is 80 DEG C, curing time 12h, is brushed with a thickness of 10mm.
Embodiment three
A kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model includes following parts by weight of component
Raw material: 100 parts of epoxy resin, 50 parts of curing agent, 23 parts of boron nitride, 7 parts of silicon carbide, 70 parts of conductive filler, silane coupling agent
1.5 parts, 6.5 parts of heat stabilizer.
The epoxy resin is bisphenol f type epoxy resin, viscosity 1500mPas, and the curing agent is solid for fatty amines
Agent, viscosity 150mPas, the boron nitride particles are spherical shape, and average grain diameter is 1 μm, and the silicon carbide is nanometer
Grade particle, average grain diameter 100nm, the conductive filler are one kind of metallic Ag and Cu, and pattern is sheet or spherical, and
Average grain diameter is 7 μm, and the silane coupling agent is γ-aminopropyl triethoxysilane and γ-(2,3- the third oxygen of epoxy) propyl
One of trimethoxy silane is a variety of, and the heat stabilizer is one of barium stearate and calcium-zinc composite stabilizing agent or more
Kind.
Preparation process specifically:
(1) it weighs conductive filler, boron nitride, silicon carbide and silane coupling agent in proportion to be mixed, and in 25 DEG C of ring
It is ultrasonically treated 1h under border, obtains composite mortar；
(2) composite mortar and epoxy resin are mixed and stirred for, revolving speed 1000rpm, time 10min；
(3) then, heat stabilizer and toughener are proportionally added into and is stirred, revolving speed 500rpm, time 5min,
(4) it is finally proportionally added into curing agent, stirs and deaeration is handled, obtain mixture；
(5) mixture is brushed and is reprinted on mould in slush mold silica gel, be placed in solidification in thermostatic drying chamber, obtain high temperature resistant
Conductive epoxy core model.
In the step (5), solidification temperature is 70 DEG C, curing time 11h, is brushed with a thickness of 7mm.
Comparative example one
Other than without using boron nitride and silicon carbide, other compositions and technique are all the same as example 1, and obtain the present invention
The conductive epoxy core model.
Comparative example two
Other than without using conductive filler sheet Ag nanoparticle and copper nanoparticle, other compositions and technique all with embodiment
Three is identical, finally obtains conductive epoxy core model of the present invention.
Experimental example
The conductive epoxy core model of the preparation described in embodiment 1-3 and comparative example 1-2 carries out surface conductivity and heat resistance is surveyed
Examination, test result such as table 1:
Table 1
| Conductivity/(S/m) | Glass transition temperature Tg/ DEG C | |
| Embodiment one | 10-4 | 205 |
| Embodiment two | 10-2 | 223 |
| Embodiment three | 10-7 | 175 |
| Comparative example one | 10-5 | 110 |
| Comparative example two | 10-12 | 139 |
Seen from table 1, when conductive filler being added in epoxy resin, the electric conductivity of final epoxy core model improves a lot.Such as
Embodiment two, when the two is arranged in pairs or groups in use, since the bridge coil of sheet Ag particle and spherical copper nanoparticle is better, at this time
The conductivity of epoxy core model is up to 10-2S/m meets performance requirement (conductivity > 10 of subsequent electroforming-4S/m).By comparing reality
It applies example 1 and comparative example 1, glass transition temperature Tg is added after boron nitride or silicon carbide in epoxy resin by 110 DEG C and is increased to 200
DEG C, improve 81.8%.
The present invention provides a kind of epoxy resin for having both high temperature resistant and electric conductivity, and are practiced in slush mold epoxy core model
Preparation so that epoxy core model have good surface conductivity, do not need carry out conductive treatment can directly carry out
Electroforming fundamentally solves deficiency existing for traditional conductive treatment technique.High temperature resistant conductive epoxy provided by the invention
Resin has the advantages that high temperature resistant, viscosity are low, and has excellent electric conductivity, finds after tested, conductivity reaches as high as 10-2S/
M meets performance requirement (conductivity > 10 of subsequent electroforming-4S/m).The preparation of high temperature resistant conductive epoxy resin provided by the invention
Method and process is simple, easy to operate.
Fig. 1 is conductive epoxy core mold structure schematic diagram, and conductive epoxy core model includes mold base, conductive layer and decorative pattern, is led
The upside of mold base is arranged in electric layer, and the upside of conductive layer is arranged in decorative pattern.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model, which is characterized in that comprising following
The raw material of parts by weight of component: 100 parts of epoxy resin, 50 parts of curing agent, 20-25 parts of boron nitride, 5-10 parts of silicon carbide, conductive filler
60-80 parts, 0.5-2 parts of silane coupling agent, 5-8 parts of heat stabilizer.
2. a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model according to claim 1,
It is characterized in that, the epoxy resin is bisphenol f type epoxy resin, viscosity 1000-2000mPas.
3. a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model according to claim 1,
It is characterized in that, the curing agent is fatty amines curing agent, viscosity 150mPas.
4. a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model according to claim 1,
It is characterized in that, the boron nitride particles are spherical shape, and average grain diameter is 1 μm.
5. a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model according to claim 1,
It is characterized in that, the silicon carbide is nanometer particle, average grain diameter 100nm.
6. a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model according to claim 1,
It is characterized in that, the conductive filler is the one or more of metallic Ag and Cu, pattern is sheet or spherical, and averagely grain
Diameter is 5-10 μm.
7. a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model according to claim 1,
It is characterized in that, the silane coupling agent is γ-aminopropyl triethoxysilane and γ-(2,3- the third oxygen of epoxy) propyl front three
One of oxysilane is a variety of.
8. a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model according to claim 1,
It is characterized in that, the heat stabilizer is one of barium stearate and calcium-zinc composite stabilizing agent or a variety of.
9. a kind of high temperature resistant conducting ring applied to the preparation of slush mold epoxy core model according to claim 1-8
Oxygen resin, which is characterized in that preparation process specifically:
(1) it weighs conductive filler, boron nitride, silicon carbide and silane coupling agent in proportion to be mixed, and in the environment of 25 DEG C
It is ultrasonically treated 1h, obtains composite mortar；
(2) composite mortar and epoxy resin are mixed and stirred for, revolving speed 1000rpm, time 10min；
(3) then, heat stabilizer and toughener are proportionally added into and is stirred, revolving speed 500rpm, time 5min,
(4) it is finally proportionally added into curing agent, stirs and deaeration is handled, obtain mixture；
(5) mixture is brushed and is reprinted on mould in slush mold silica gel, be placed in solidification in thermostatic drying chamber, obtain high temperature resistant conduction
Epoxy core model.
10. a kind of high temperature resistant conductive epoxy resin applied to the preparation of slush mold epoxy core model according to claim 9,
It is characterized in that, solidification temperature is 60-80 DEG C, curing time 10-12h in the step (5), brush with a thickness of 5-10mm.
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| CN111519217A (en) * | 2020-05-07 | 2020-08-11 | 吉林大学 | Slush molding die and reinforcement treatment method and application thereof |
| CN112080095A (en) * | 2020-09-11 | 2020-12-15 | 成都玉龙化工有限公司 | Modified PVB resin and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111519217A (en) * | 2020-05-07 | 2020-08-11 | 吉林大学 | Slush molding die and reinforcement treatment method and application thereof |
| CN112080095A (en) * | 2020-09-11 | 2020-12-15 | 成都玉龙化工有限公司 | Modified PVB resin and preparation method thereof |
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Application publication date: 20191008 |