CN106084669A - A kind of organic siliconresin modified epoxy resin composition - Google Patents
A kind of organic siliconresin modified epoxy resin composition Download PDFInfo
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- CN106084669A CN106084669A CN201610446068.1A CN201610446068A CN106084669A CN 106084669 A CN106084669 A CN 106084669A CN 201610446068 A CN201610446068 A CN 201610446068A CN 106084669 A CN106084669 A CN 106084669A
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- epoxy resin
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- silicones
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
- C08L63/04—Epoxynovolacs
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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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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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a kind of organic siliconresin modified epoxy resin composition, mainly comprise for: in terms of parts by weight, epoxy resin 100 parts, organic siliconresin 0.3 80 parts, organic siliconresin solubilizing agent 5 80 parts, diethyl toluene diamine 19.58 parts.The organic siliconresin modified epoxy resin composition of the present invention, containing a kind of organic siliconresin with double-deck closely chondritic, can be with epoxy resin fully compatible under organic siliconresin solubilizing agent effect, be dispersed in epoxy resin in, the fire resistance making co-mixing system is greatly improved, and strengthens flame retardant effect.
Description
Technical field
The present invention relates to a kind of composition epoxy resin, more specifically to one change containing organic silicon resin fire retardant
The compositions of property epoxy resin.
Background technology
Epoxy resin is extensively applied as matrix resin in the composite, is the thermosetting tree of a class function admirable
Fat, but be readily burned and limit its use in some field.Therefore, molding for epoxy resin have employed substantial amounts of fire retardant,
Such as halogen contained compound, boron derivative, metal-oxide, phosphorus-containing compound etc., can singly add or compounding.But, chloride and bromine
Fire proofing easily release when burning there is zest and corrosive hydrogen halide, therefore halogen flame is the most gradually
It is restricted；In order to avoid the harm using traditional halogenated flame retardant to bring environment, people are devoted to develop Halogen now
Fire retardant.Conventional phosphorous, compound that nitrogen class is fire-retardant, can cause again ecological problem.Organic silicon resin fire retardant both can carry
The anti-flammability of high matrix, can improve again the heat stability of resin.Compared with other fire retardant such as halogen system, phosphorus system etc., silicon system hinders
Combustion agent has the performance of its excellence: Heat stability is good, low burn rate, low thermal discharge, anti-drippage and low cigarette, low CO give birth to
The performances such as Cheng Liang.Modifying epoxy resin by organosilicon can improve the mechanical performance of resin, as reduce internal stress of resin, increase its break
Split percentage elongation and toughness；Can increase again the chemical property of resin, such as resistance to oxidation, thermostability etc., these all make organic silicon flame-retardant
Agent receives much concern, but organic silicon resin fire retardant and epoxy resin still suffer from consistency problem.
Summary of the invention
It is an object of the invention to provide a kind of organic siliconresin with double-deck closely chondritic, increase at organic siliconresin
Under solvent action can with epoxy resin fully compatible, be dispersed in epoxy resin in, make co-mixing system fire-retardant
Performance is greatly improved.
One organic siliconresin modified epoxy resin composition of the present invention, mainly comprise for: in terms of parts by weight,
The organic siliconresin modified epoxy resin composition of the present invention, wherein, described epoxy resin is glycidyl ether
Class, aromatic series or aliphatic epoxy resin.
The organic siliconresin modified epoxy resin composition of the present invention, wherein, described epoxy resin is epoxy novolac tree
Fat.
The organic siliconresin modified epoxy resin composition of the present invention, wherein, described silicones is methyl MQ silicones.
The organic siliconresin modified epoxy resin composition of the present invention, wherein, described silicones is that bilayer is the most spherical
The methyl MQ silicones of structure.
The organic siliconresin modified epoxy resin composition of the present invention, wherein, described organic siliconresin solubilizing agent, use
Following method synthesizes: by 23.6g γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and 18g dimethyldimethoxysil,ne
And appropriate dehydrated alcohol puts into the 250ml round bottom three-necked bottle being provided with agitator, thermometer and reflux condensing tube, at 50 DEG C
Waters pot stirs 30 minutes；Then in three-necked bottle, add 7.56g deionized water and 0.4g ammonia.Stirring reaction at 50 DEG C
4.5 hours, finally add appropriate 1-chlorine trimethyl silane and react 1 hour, after terminating, products therefrom is placed in equipped with just own
Precipitated and separated in the beaker of alkane, collects lower floor's solution and removes unreacted material；Lower floor's solution carries out rotation steam, until free from admixture
Steam, finally obtain light yellow viscous liquid product.
The method have the advantages that
Using the methyl MQ silicones of double-deck closely chondritic as fire retardant in the present invention, methyl MQ silicones is one
The polyorganosiloxane resin that class is special, by Mono-functional siloxanes's unit (R3SiO1/2 is called for short M) and four-functional group siloxane unit
(SiO4/2 is called for short Q) composition., MQ silicones outward appearance be the tight spheroid of double-decker, i.e. core part be Si-O-Si chain even
Connecing, caged SiO2 that density is higher and the degree of polymerization is 15～50, spherical shell is the R3SiO1/2 layer that density is less, MQ silicones big
Part chain end hydroxyl is all replaced by R3SiO1/2；Ethoxyline resin antiflaming can be improved, and make in organic siliconresin solubilizing agent
With lower the best with the compatibility of epoxy resin, it be applicable to the overwhelming majority and plant based epoxy resin, with its fire-retardant epoxy resin
The homogeneous bubble-free of casting resin.
Detailed description of the invention
By the following examples the present invention is further described specifically.Be necessary it is pointed out here that be following enforcement
Example is served only for that the present invention is described further, it is impossible to being interpreted as limiting the scope of the invention, this art is ripe
Practice personnel, according to the invention described above content, the present invention is made some nonessential improvement and adjustment, still fall within the protection of the present invention
Scope.
Embodiment 1
Prepared by composition epoxy resin: by novolac epoxy resin (epoxide number 0.51mol/100g, Shanghai resin company limited
F-51) 100 parts are heated to 80 DEG C, add organic siliconresin solubilizing agent 10 parts, low rate mixing 0.5 hour, add double-deck closely ball
The methyl MQ silicones (technical grade Zhonglan Chenguang Chemical Inst) 0.3 part of shape structure, diethyl toluene diamine 19.58 parts, treat
After stirring, it is poured in the mould of preheating (for preventing silicones from solidifying, this step must complete in 15 minutes).Connect
And be heating and curing in the air dry oven of preference temperature, temperature is 130 DEG C/2.5 hours, 160 DEG C/2.5 hours. after solidification i.e.
Obtain fire-retardant epoxy resin fat solidfied material.
Prepared by organic siliconresin solubilizing agent: by 23.6g γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane (KH560)
Put into 18g dimethyldimethoxysil,ne (DEMS) and appropriate dehydrated alcohol and agitator, thermometer and returned cold are installed
The 250ml round bottom three-necked bottle of solidifying pipe, stirs 30 minutes in the waters pot of 50 DEG C.Then in three-necked bottle add 7.56g go from
Sub-water and 0.4g ammonia.Stirring reaction 4.5 hours at 50 DEG C.Finally adding appropriate 1-chlorine trimethyl silane, to react 1 little
Time.After end, products therefrom is placed in equipped with precipitated and separated in the beaker of normal hexane, collects lower floor's solution and remove unreacted thing
Matter.Lower floor's solution carries out rotation steam, until free from admixture steams, finally obtain light yellow viscous liquid product, preserve stand-by, below
Embodiment is identical.
Embodiment 2
Composition epoxy resin: by novolac epoxy resin (epoxide number 0.51mol/100g, Shanghai resin company limited F-
51) 100 parts are heated to 80 DEG C, add organic siliconresin solubilizing agent (same as in Example 1) 10 parts, low rate mixing 0.5 hour, add
Enter to have double-deck closely the methyl MQ silicones 0.5 part of chondritic, diethyl toluene diamine 19.58 parts, to be mixed uniformly after,
It is poured in the mould of preheating (for preventing silicones from solidifying, this step must complete in 15 minutes).Then in suitable temperature
Being heating and curing in the air dry oven of degree, temperature is 130 DEG C/2.5 hours, 160 DEG C/2.5 hours. i.e. obtain flame retardant type ring after solidification
Epoxy resins fat solidfied material.
Embodiment 3
Composition epoxy resin: by novolac epoxy resin (epoxide number 0.51mol/100g, Shanghai resin company limited F-
51) 100 parts are heated to 80 DEG C, addition laboratory research and development organic siliconresin solubilizing agent (HPSi) 10 parts, low rate mixing 0.5 hour,
Add and there is double-deck closely the methyl MQ silicones 1 part of chondritic, diethyl toluene diamine 19.58 parts, to be mixed uniformly after,
It is poured in the mould of preheating (for preventing silicones from solidifying, this step must complete in 15min).Then in preference temperature
Air dry oven in be heating and curing, temperature is 130 DEG C/2.5 hours, 160 DEG C/2.5 hours. i.e. obtain flame retardant type epoxy after solidification
Resin ester solidfied material.
Embodiment 4
Composition epoxy resin: by novolac epoxy resin (epoxide number 0.51mol/100g, Shanghai resin company limited F-
51) 100 parts are heated to 80 DEG C, organic siliconresin solubilizing agent 10 parts, low rate mixing 0.5 hour, and it is the most spherical that addition has bilayer
The methyl MQ silicones 3 parts of structure, diethyl toluene diamine 19.58 parts, to be mixed uniformly after, be poured in the mould of preheating
(for preventing silicones from solidifying, this step must complete in 15min).Then in the air dry oven of preference temperature, add thermosetting
Changing, temperature is 130 DEG C/2.5 hours, 160 DEG C/2.5 hours. i.e. obtain fire-retardant epoxy resin fat solidfied material after solidification.
Embodiment 5
Composition epoxy resin: by novolac epoxy resin (epoxide number 0.51mol/100g, Shanghai resin company limited F-
51) 100 parts are heated to 80 DEG C, addition laboratory research and development organic siliconresin solubilizing agent (HPSi) 10 parts, low rate mixing 0.5 hour,
Add and there is double-deck closely the methyl MQ silicones 5 parts of chondritic, diethyl toluene diamine (DETDA) 19.58 parts, to be mixed
After Jun Yun, it is poured in the mould of preheating (for preventing silicones from solidifying, this step must complete in 15min).Then exist
Being heating and curing in the air dry oven of preference temperature, temperature is 130 DEG C/2.5 hours, 160 DEG C/2.5 hours. i.e. obtain resistance after solidification
Combustion type epoxy resin fat solidfied material.
Methyl MQ resin/epoxy resin diethyl toluene diamine system anti-flammability and thermostability test result such as following table.Pole
The mensuration of limited oxygen index: refer in XYC-75 oxygen according to GB GB/T2406-93 (Plastics Combustion performance test methods: oxygen index method)
Measure its fire resistance and record its combustion characteristics on number analyzer.
Vertical combustion performance measures: promulgate vertical combustion standard testing according to Underwriter Laboratory Inc..
Often organize at least 5 standard battens to test.
Claims (8)
1. an organic siliconresin modified epoxy resin composition, mainly comprise for: in terms of parts by weight,
2., according to the composition epoxy resin described in claim 1, it is characterised in that wherein, described epoxy resin is for shrinking
Glycerol ethers, aromatic series or aliphatic epoxy resin.
3., according to the composition epoxy resin described in claim 1, it is characterised in that wherein, described epoxy resin is phenolic aldehyde
Epoxy resin.
4., according to the composition epoxy resin described in claim 1, it is characterised in that wherein, described silicones is methyl MQ
Silicones.
5., according to the composition epoxy resin described in claim 1 or 4, it is characterised in that wherein, described silicones is double-deck
The closely methyl MQ silicones of chondritic.
6. according to the composition epoxy resin described in claim 1, it is characterised in that wherein, described organic siliconresin solubilising
Agent, uses following method to synthesize: by 23.6g γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and 18g dimethylformamide dimethyl
TMOS and appropriate dehydrated alcohol put into the 250ml round bottom three-necked bottle being provided with agitator, thermometer and reflux condensing tube,
The waters pot of 50 DEG C stirs 30 minutes；Then in three-necked bottle, add 7.56g deionized water and 0.4g ammonia；At 50 DEG C
Stirring reaction 4.5 hours, finally adds appropriate 1-chlorine trimethyl silane and reacts 1 hour, be placed in by products therefrom after terminating
Equipped with precipitated and separated in the beaker of normal hexane, collect lower floor's solution and remove unreacted material；Lower floor's solution carries out rotation steam, directly
Steam to free from admixture, finally obtain light yellow viscous liquid product.
7. according to the composition epoxy resin described in claim 1, it is characterised in that wherein, novolac epoxy resin 100 parts, double
The methyl MQ silicones 3 parts of layer closely chondritic, organic siliconresin solubilizing agent 10 parts, diethyl toluene diamine 19.58 parts.
8. according to the composition epoxy resin described in claim 1, it is characterised in that wherein, novolac epoxy resin 100 parts, double
The methyl MQ silicones 0.5 part of layer closely chondritic, organic siliconresin solubilizing agent 10 parts, diethyl toluene diamine 19.58 parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610446068.1A CN106084669A (en) | 2016-06-21 | 2016-06-21 | A kind of organic siliconresin modified epoxy resin composition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610446068.1A CN106084669A (en) | 2016-06-21 | 2016-06-21 | A kind of organic siliconresin modified epoxy resin composition |
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| Publication Number | Publication Date |
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| CN106084669A true CN106084669A (en) | 2016-11-09 |
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| CN201610446068.1A Pending CN106084669A (en) | 2016-06-21 | 2016-06-21 | A kind of organic siliconresin modified epoxy resin composition |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864924A (en) * | 2018-07-04 | 2018-11-23 | 湖北恒驰电子科技有限公司 | A kind of halogen-free resin composition and the flexible printed-circuit board cover film prepared with it |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01225621A (en) * | 1988-03-07 | 1989-09-08 | Hitachi Chem Co Ltd | Epoxy resin composition |
| JP2005171166A (en) * | 2003-12-15 | 2005-06-30 | Sanyo Chem Ind Ltd | Casting resin composition |
| JP2006008747A (en) * | 2004-06-22 | 2006-01-12 | Nippon Kayaku Co Ltd | Epoxy compound and thermosetting resin composition |
| CN102977553A (en) * | 2012-11-06 | 2013-03-20 | 中科院广州化学有限公司 | Epoxy/silicone polymer composite material, and preparation method and application thereof |
-
2016
- 2016-06-21 CN CN201610446068.1A patent/CN106084669A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01225621A (en) * | 1988-03-07 | 1989-09-08 | Hitachi Chem Co Ltd | Epoxy resin composition |
| JP2005171166A (en) * | 2003-12-15 | 2005-06-30 | Sanyo Chem Ind Ltd | Casting resin composition |
| JP2006008747A (en) * | 2004-06-22 | 2006-01-12 | Nippon Kayaku Co Ltd | Epoxy compound and thermosetting resin composition |
| CN102977553A (en) * | 2012-11-06 | 2013-03-20 | 中科院广州化学有限公司 | Epoxy/silicone polymer composite material, and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864924A (en) * | 2018-07-04 | 2018-11-23 | 湖北恒驰电子科技有限公司 | A kind of halogen-free resin composition and the flexible printed-circuit board cover film prepared with it |
| CN108864924B (en) * | 2018-07-04 | 2020-10-27 | 湖北恒驰电子科技有限公司 | Halogen-free resin composition and cover film for flexible printed circuit board prepared from same |
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Application publication date: 20161109 |