CN105566679A - Ester compound, and preparation method and application thereof to epoxy resin casting system - Google Patents
Ester compound, and preparation method and application thereof to epoxy resin casting system Download PDFInfo
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- CN105566679A CN105566679A CN201511008664.3A CN201511008664A CN105566679A CN 105566679 A CN105566679 A CN 105566679A CN 201511008664 A CN201511008664 A CN 201511008664A CN 105566679 A CN105566679 A CN 105566679A
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- anhydride
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
-
- 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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
-
- 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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3324—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof cyclic
- C08G65/3326—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof cyclic aromatic
-
- 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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/48—Polymers modified by chemical after-treatment
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
-
- 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
Abstract
An ester compound has both a flexible structure and a rigid structure, and is prepared by reaction of 30-60 parts of divalent alcohol and polyhydric alcohol, and 30-60 parts of divalent alcohol and polybasic carboxylic acid or anhydride. The ester compound of the invention is applicable to a casting system made of epoxy resin, and can reduce the volume shrinkage ratio (volume shrinkage ratio of 1% to 2%) of the system, improve the resistance to cracking, and significantly reduce the glass transition temperature (100-120 DEG C) of the uncured products. The ester compound overcomes the shortcomings of high shrinkage and low glass transition temperature of the products in the market, and can be used in the fields of indoor and outdoor (especially in the environment with large temperature difference) middle and high-voltage electrical equipment castable, encapsulation material of electronic packaging materials, and potting materials.
Description
Technical field
The present invention relates to a kind of ester cpds, particularly relate to a kind of cold coating, there is high rigidity, light, thermofixation condition can be met.
Background technology
Epoxy resin is as encapsulation and the field such as adhesive backers widespread use electronics and electrical equipment.Owing to containing a large amount of epoxide groups in its molecule, epoxy resin after hardening cross-linking density is high, lacks slip between molecular chain, internal stress is large, cause curing material embrittlement, very easily occur cracking phenomena, this has become one of principal element that limit collar oxygen product further develops.According to the molecular theory of fracture, the stress concentration that the fracture of material comes from internal stress distribution inequality and causes.
For curable epoxide thing, the reason of internal stress skewness mainly comes from 2 points: be due to liberated heat skewness during solidification on the one hand; Because thermal expansivity is different on the other hand.
The solidification of epoxy resin belongs to thermopositive reaction, the stress concentration that during solidification, liberated heat skewness causes.In solidify reaction process, heat release is more, more easily causes concentrating of thermal stresses.Meanwhile, liberated heat will speed up the thermal motion of molecule, accelerates rate of crosslinking, causes partial cross-linking to spend height, and then cause stress concentration.
The metal inserts such as copper, aluminium, iron core and coil are often inlayed, because resin and these metals have different thermal expansivity, if design unreasonable or misoperation all will cause stress distribution inequality in pouring piece.For epoxy resin, caused by the contraction of internal stress mainly glass region, and substantially do not produce when elastomeric state.
The size of internal stress depends primarily on the size of shrinking percentage, by the linearly ratio rising of the decline along with temperature under vitreous state.Therefore, reducing shrinking percentage is one of important means improving epoxy material splitting resistance.
In general, volumetric shrinkage during epoxy resin cure is more than 5%.The method reducing volumetric shrinkage has following several usually: the methods such as appropriate design molecular structure, reduction Tg, interpolation mineral filler and introducing toughner.The common method of current solution epoxy resin splitting resistance introduces the toughner with flexible chain structure.But the method often causes the second-order transition temperature (Tg) of cured article to decline, with the performance such as thermotolerance and intensity of sacrificing epoxy resin for cost improves toughness of material.For the epoxy casting glue being applied to high-voltage electrical apparatus industry, the Tg of home products is generally lower than same kind of products at abroad.For dry type transformer epoxy casting glue, in the Multiple Type product of certain external producer, Tg reaches as high as 110 DEG C ~ 120 DEG C.But the Tg of main products common on market is scarcely higher than 80 DEG C.Therefore, exploitation has the neo-epoxy resin casting system of high Tg lower shrinkage, solves Tg this Key technique problem too low of domestic epoxy casting glue, has important practice and scientific meaning.
Summary of the invention
One object of the present invention is to provide a kind of ester cpds, is applicable to the casting system of epoxy resin composition.
Another object of the present invention is to provide a kind of ester cpds as toughner for epoxy resin, reduces the volumetric shrinkage of system, improves splitting resistance.
Another object of the present invention is the preparation method providing a kind of ester cpds, to obtain ester cpds.
Another object of the present invention is to provide one to build composition, has level and the comparatively low-shrinkage of higher Tg, is suitable as high voltage electric equipment mould material and electronic encapsulation material.
For achieving the above object, a kind of ester cpds provided by the invention, by weight, comprising:
30 ~ 60 parts of binary and the above polyvalent alcohol of binary, and 30 ~ 60 parts of binary and the above polycarboxylic acid of binary or acid anhydrides.
Binary and the above polyvalent alcohol of binary as: but be not limited only to glycol ether, Triethylene glycol, polyether Glycols, polyether glycol, C
nh
2n+2-m(OH)
mone or more of (n>=3, m>=2), and binary and the above aromatic polyol of binary as: but be not limited only to terephthalyl alcohol, phthalyl alcohol, isophthalic alcohol, 1,3,5-benzene three methyl alcohol and Isosorbide-5-Nitrae-benzene di-alcohol etc.These compounds are applied to the present invention alone or in combination.
Binary and the above polycarboxylic acid of binary are as formula C
xh
2x+2-y(COOH)
y(x>=3, y>=2) shown in one or more of compound, and binary and the above aromatic polycarboxylic acid of binary as: but be not limited only to terephthalic acid, phthalic acid, m-phthalic acid, trimesic acid, Pyromellitic Acid, to phenylene-diacetic acid, phthalic acid and a phenylene-diacetic acid etc.These carboxylic acids are applied to the present invention alone or in combination.
Acid anhydrides be aromatic anhydride as: but be not limited only to Tetra hydro Phthalic anhydride, trimellitic anhydride, pyromellitic acid anhydride and Benzophenone carboxylic acid dianhydride etc., and formula C
ph
2p+2-q(COCOO)
qone or more of compound shown in (p>=3, q>=2).These acid anhydrides are applied to the present invention alone or in combination.
Another kind of ester cpds provided by the invention, by weight, comprising:
30 ~ 60 parts of binary and the above polyvalent alcohol of binary, and 30 ~ 60 parts of binary and the above polycarboxylic acid of binary or acid anhydrides, wherein binary and the above polyvalent alcohol of binary are selected from glycol ether, Triethylene glycol, polyether Glycols, polyether glycol and C
nh
2n+2-m(OH)
mone or more of (n>=3, m>=2), the structure of these alcohol presents flexibility; Binary and the above polycarboxylic acid of binary are selected from binary and above aromatic polycarboxylic acid; Acid anhydrides is aromatic anhydride, and the structure of these acid presents rigidity.
Another kind of ester cpds provided by the invention, by weight, comprising:
30 ~ 60 parts of binary and the above polyvalent alcohol of binary, and 30 ~ 60 parts of binary and the above polycarboxylic acid of binary or acid anhydrides, wherein binary and the above polyvalent alcohol of binary are selected from binary and the above aromatic polyol of binary; Binary and the above polycarboxylic acid of binary are selected from formula C
xh
2x+2-y(COOH) one or more of compound shown in y (x>=3, y>=2); Acid anhydrides is selected from formula C
ph
2p+2-q(COCOO)
qone or more of compound shown in (p>=3, q>=2).
The preparation method of a kind of ester cpds provided by the invention, it comprises the steps:
First by 30 ~ 60 weight part binary and the above polyvalent alcohol of binary, and 30 ~ 60 weight part binary and the above polycarboxylic acid of binary or acid anhydrides add in container, are warming up to 80 DEG C ~ 100 DEG C, stir, make it fully mix;
After abundant mixing, be warming up to 170 DEG C ~ 220 DEG C with the speed of 2 DEG C ~ 5 DEG C/min, distillate until no longer include water molecules, stopped reaction;
Finally, cooling, discharging, obtains light yellow clear liquid.
The ester cpds that the present invention obtains is applicable to, with the casting system of epoxy resin composition, can be used as toughner for epoxy resin, reduces the volumetric shrinkage of system, improves splitting resistance.
One provided by the invention builds composition, by weight, comprising:
One provided by the invention builds composition, by weight, comprises the first component and second component, wherein
First component comprises:
Epoxy resin 20 ~ 50
Ester cpds 5 ~ 30
Filler 30 ~ 80;
Second component comprises:
Acid anhydride type curing agent 15 ~ 45
Curing catalyst 0.01 ~ 0.3
Filler 30 ~ 80.
Provided by the inventionly build composition, the oxirane value of epoxy resin used is 0.105eq/100g ~ 1.000eq/100g.
Provided by the inventionly build composition, acid anhydride type curing agent used is selected from aromatic anhydride, one of aliphatic anhydride and alicyclic acid anhydrides are planted or several.Wherein, aromatic anhydride as: but be not limited only to Tetra hydro Phthalic anhydride and affixture, trimellitic anhydride and affixture thereof, pyromellitic acid anhydride and affixture thereof and 3,3 ', 4,4 '-Benzophenone carboxylic acid dianhydride and affixture etc. thereof, these acid anhydrides can be used alone or Combination application in the present invention.Aliphatic anhydride as: but be not limited only to poly-nonane diacid acid anhydride, poly sebacic polyanhydride and poly-petrosilane diacid anhydride etc., these acid anhydrides can be used alone or Combination application in the present invention.Alicyclic acid anhydrides as: but be not limited only to MALEIC ANHYDRIDE, tung oil acid anhydride, tetrahydrochysene phthalate anhydride, methyl tetrahydrochysene phthalate anhydride, hexahydrophthalic acid anhydride, methyl hexahydrophthalic acid anhydride, carbic anhydride and methylnadic anhydride etc., these acid anhydrides can be used alone or Combination application in the present invention.
Provided by the inventionly build composition, ester cpds used, the binary contained by it and molecular weight more than binary are 60Da ~ 3,000Da.
Provided by the inventionly build composition, curing catalyst used as: but be not limited only to benzyldimethylamine, 2,4,6-tri-(dimethylamino methyl) phenol, N, accelerine, diethyl amino propylamine, 2-ethyl-4-methylimidazole, methyl ethyl diketone network, zinc acetylacetonate, benzyl trimethyl ammonium chloride, trolamine borate, triethanol amine titanate, triphenylphosphine and salt, 1 thereof, 8-diaza-dicyclo (5,4,0)-7-undecylene and organic salt and 2-benzylimidazoline etc., these compounds can be used alone or Combination application in the present invention.
Provided by the inventionly build composition, filler used as: but be not limited only to silica flour, aluminum oxide, aluminium hydroxide, magnesium hydroxide, barium sulfate, calcium carbonate, boron nitride and aluminium nitride etc., these materials are applied to the present invention alone or in combination, median size prioritizing selection 1 μm ~ 50 μm.
Provided by the inventionly build composition, have level (100 DEG C ~ 120 DEG C) and the comparatively low-shrinkage (volumetric shrinkage is 1% ~ 2%) of higher Tg, volume specific resistance is for being about (1.0 ~ 9.0) × 10
13Ω m.It is as cured article, is suitable as mesohigh electric installation mould material and electronic encapsulation material.
The preparation method building composition provided by the invention, first produces the first component and the second composition respectively, then by the first component and second component mixing, wherein
Prepare the first component: in temperature 70 C ~ 80 DEG C, stir 500r/min ~ 1500r/min and vacuum tightness 0.07MPa ~ 0.13MPa condition under, by weight, epoxy resin 20 ~ 50, ester cpds 5 ~ 30 and filler 30 ~ 80 are mixed, time 2 h ~ 3 hour;
Prepare second component: under temperature 65 DEG C ~ 75 DEG C, stirring 500r/min ~ 1500r/min and vacuum tightness 0.07MPa ~ 0.13MPa condition, by weight, anhydride curing agent 15 ~ 45, curing catalyst 0.01 ~ 0.3 and filler 30 ~ 80 are mixed, time 2 h ~ 3 hour.
Batch mixing: in temperature 70 C ~ 80 DEG C, under stirring 500r/min ~ 1500r/min and vacuum tightness 0.07MPa ~ 0.13MPa condition, mixes the first component and second component.
Composition deaeration to be built is clean, can carry out cast cured explosive.
In the present invention, alleged " binary and the above polyvalent alcohol of binary " should be understood to comprise: be used alone dibasic alcohol or the above polyvalent alcohol of binary, and uses the situation of dibasic alcohol and the above polyvalent alcohol of binary simultaneously.
In the present invention, alleged " binary and the above polycarboxylic acid of binary " should be understood to comprise: be used alone di-carboxylic acid or the above polycarboxylic acid of binary, and uses the situation of di-carboxylic acid and the above polycarboxylic acid of binary simultaneously.
The beneficial effect that technical solution of the present invention realizes:
Ester cpds provided by the invention, it is a kind of compound simultaneously with flexible structure and rigid structure, be applicable to the casting system of epoxy resin composition, the volumetric shrinkage of system can be reduced, improve splitting resistance, the second-order transition temperature of cured article is not made significantly to reduce, overcome the high and shortcoming that second-order transition temperature is on the low side of related products shrinking percentage on market, can be used for the field such as encapsulating material, potting compound in indoor, outdoor (particularly at the environment that the temperature difference is larger) mesohigh electric installation mould material, electronic package material.
Provided by the inventionly building composition, is poured with epoxy resin material, can be used as two-pack and uses, and has that viscosity is low, working life long, a feature such as workable and applied range.
Embodiment
Below describe technical scheme of the present invention in detail.The embodiment of the present invention is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to the technical scheme of invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in right of the present invention.
The key step of the ester cpds that following examples of the present invention are produced is as follows:
Reactant is added in the there-necked flask that heating jacket, agitator, thermometer and prolong are housed, is warming up to 80 DEG C ~ 100 DEG C, stir, make it fully mix; Subsequently, be slowly warming up to 170 DEG C ~ 220 DEG C, distillate until no longer include water molecules, stopped reaction, obtain light yellow clear liquid, be i.e. ester cpds of the present invention.
Following examples of the present invention produce casting composition key step as follows:
Prepare the first component: in temperature 70 C ~ 80 DEG C, stir 500r/min ~ 1500r/min and vacuum tightness 0.07MPa ~ 0.13MPa condition under, by weight, by epoxy resin (purchased from Yueyang petrochemical industry epoxy resin factory, CYD-128), ester cpds and filler (particle diameter 10 μm ~ 20 μm) mix, time 2 h ~ 3 hour;
Prepare second component: under temperature 65 DEG C ~ 75 DEG C, stirring 500r/min ~ 1500r/min and vacuum tightness 0.07MPa ~ 0.13MPa condition, by weight, anhydride curing agent, curing catalyst and filler (particle diameter 10 μm ~ 20 μm) are mixed, time 2 h ~ 3 hour.
Batch mixing: in temperature 70 C ~ 80 DEG C, under stirring 500r/min ~ 1500r/min and vacuum tightness 0.07MPa ~ 0.13MPa condition, mixes the first component and second component.
Embodiment 1
By taking following component shown in table 1 and correspondingly producing ester cpds.
Table 1
After testing, obtained ester cpds is liquid, and pH value is between 6.5 ~ 7.5, and viscosity is 600mPa.s ~ 2000mPa.s.Mixed in mass ratio as toughner with epoxy resin by such ester cpds, the second-order transition temperature (Tg/ DEG C) of gained cured article reduces with the increase of ester cpds consumption, but reduction degree is far smaller than commercially available toughner, as shown in Table 2 below.
Table 2
Embodiment 2
By taking following component shown in table 3 and correspondingly producing casting system, commercially available toughner is made by identical preparation method simultaneously and think comparative example.
Table 3
By obtained build composition bubble removing after pour into a mould, condition of cure is: 4 hours ~ 6 hours 80 DEG C, then 3 hours ~ 5 hours 110 DEG C, last 8 hours ~ 10 hours 130 DEG C, and detect by method shown in table 6, detected result is in table 5.
From detection, the ester cpds that the present embodiment obtains is as toughner, produce epoxy resin and build composition, in volumetric shrinkage, flexural strength, elongation at break and cold-hot number of shocks etc., be all better than, with the obtained similar casting system of commercially available toughner, there is excellent anti-cracking performance.
Table 5
Table 6
| Test item | Detection method |
| Volumetric shrinkage | ISO 3521-1997 |
| Hardness | D type Shore durometer |
| Flexural strength, MPa | GB/T 9341-2008 |
| Tensile strength, MPa | GB/T 1040-2006 |
| Elongation at break, % | GB/T 1040-2006 |
| Volume specific resistance, Ω m | GB/T1410-2006 |
| Surface resistivity, Ω | GB/T1410-2006 |
Claims (27)
1. an ester cpds, by weight, comprises 30 ~ 60 parts of binary and the above polyvalent alcohol of binary, and 30 ~ 60 parts of binary and the above polycarboxylic acid of binary or acid anhydrides;
Described binary and the above polyvalent alcohol of binary are selected from glycol ether, Triethylene glycol, polyether Glycols, polyether glycol and formula C
nh
2n+2-m(OH)
mone or more, and binary and the above aromatic polyol of binary, wherein n>=3, m>=2;
Described binary and the above polycarboxylic acid of binary are formula C
xh
2x+2-y(COOH)
yshown in one or more of compound, and one or more of binary and the above aromatic polycarboxylic acid of binary, wherein x>=3, y>=2;
Acid anhydrides is one or more of aromatic anhydride, and general formula C
ph
2p+2-q(COCOO)
qshown in one or more of compound, wherein p>=3, q>=2.
2. ester cpds according to claim 1, is characterized in that described binary and the above polyvalent alcohol of binary are selected from glycol ether, Triethylene glycol, polyether Glycols, polyether glycol and C
nh
2n+2-m(OH)
mone or more, wherein n>=3, m>=2; Described binary and the above polycarboxylic acid of binary are binary and the above aromatic polycarboxylic acid of binary; Described acid anhydrides is selected from aromatic anhydride.
3. ester cpds according to claim 1, is characterized in that described binary and the above polyvalent alcohol of binary are selected from binary and the above aromatic polyol of binary; Binary and the above polycarboxylic acid of binary are selected from formula C
xh
2x+2-y(COOH)
yshown in one or more of compound, wherein x>=3, y>=2; Acid anhydrides is selected from formula C
ph
2p+2-q(COCOO)
qshown in one or more of compound, wherein p>=3, q>=2.
4. ester cpds according to claim 1, is characterized in that described general formula C
nh
2n+2-m(OH)
mbe selected from ethylene glycol, 1,2-propylene glycol, 1,3-PD, 1,2-butyleneglycol, 1,3-butyleneglycol, BDO, neopentyl glycol, isoprene, glycerol, trihydroxybutane, penta triol, triol, heptan triol, pungent triol, the ninth of the ten Heavenly Stems triol and one or more of butantetraol.
5. ester cpds according to claim 1, it is characterized in that described binary and the above aromatic polyol of binary be selected from terephthalyl alcohol, phthalyl alcohol, isophthalic alcohol, 1,3,5-benzene three methyl alcohol, Isosorbide-5-Nitrae-benzene di-alcohol one or more.
6. ester cpds according to claim 1, it is characterized in that described binary and the above aromatic polycarboxylic acid of binary be selected from terephthalic acid, phthalic acid, m-phthalic acid, trimesic acid, Pyromellitic Acid, to phenylene-diacetic acid, one of phthalic acid and a phenylene-diacetic acid plant or several.
7. ester cpds according to claim 1, is characterized in that described aromatic anhydride is selected from one or more of Tetra hydro Phthalic anhydride, trimellitic anhydride, pyromellitic acid anhydride and Benzophenone carboxylic acid dianhydride.
8. ester cpds according to claims 1 to 7 is used for toughner.
9. ester cpds according to claims 1 to 7 is used for epoxy resin casting system as toughner.
10. produce a method for the ester cpds described in claim 1 ~ 7, comprise the steps:
First by 30 ~ 60 weight part binary and the above polyvalent alcohol of binary, and 30 ~ 60 weight part binary and the above polycarboxylic acid of binary or acid anhydrides add in container, are warming up to 80 DEG C ~ 100 DEG C, stir, make it fully mix;
After abundant mixing, be warming up to 170 DEG C ~ 220 DEG C with 2 DEG C ~ 5 DEG C/min, distillate until no longer include water molecules, stopped reaction; Finally, cooling, discharging, obtains light yellow clear liquid.
Build composition, it is characterized in that for 11. 1 kinds, by weight, comprising:
12. according to claim 11ly build composition, it is characterized in that comprising the first component and second component, wherein
The first described component comprises:
Epoxy resin 20 ~ 50
Ester cpds 5 ~ 30
Filler 30 ~ 80;
Described second component comprises:
Acid anhydride type curing agent 15 ~ 45
Curing catalyst 0.01 ~ 0.3
Filler 30 ~ 80.
13. according to claim 11ly build composition, it is characterized in that the oxirane value of described epoxy resin is 0.105eq/100g ~ 1.000eq/100g.
14. according to claim 11ly build composition, it is characterized in that described acid anhydride type curing agent is selected from aromatic anhydride, one of aliphatic anhydride and alicyclic acid anhydrides are planted or several.
15. according to claim 11ly build composition, it is characterized in that described acid anhydride type curing agent is selected from Tetra hydro Phthalic anhydride and affixture, trimellitic anhydride and affixture thereof, pyromellitic acid anhydride and affixture thereof and 3,3 ', 4, one or more of 4 '-Benzophenone carboxylic acid dianhydride and affixture thereof.
16. according to claim 11ly build composition, it is characterized in that described acid anhydride type curing agent is selected from one or more of poly-nonane diacid acid anhydride, poly sebacic polyanhydride and poly-petrosilane diacid anhydride.
17. according to claim 11ly build composition, it is characterized in that described acid anhydride type curing agent is selected from one or more of MALEIC ANHYDRIDE, tung oil acid anhydride, tetrahydrochysene phthalate anhydride, methyl tetrahydrochysene phthalate anhydride, hexahydrophthalic acid anhydride, methyl hexahydrophthalic acid anhydride, carbic anhydride and methylnadic anhydride.
18. according to claim 11ly build composition, it is characterized in that the molecular weight of more than the binary that described ester cpds contains and binary is 60Da ~ 3,000Da.
19. according to claim 11ly build composition, it is characterized in that described curing catalyst is selected from benzyldimethylamine, 2,4,6-tri-(dimethylamino methyl) phenol, N, accelerine, diethyl amino propylamine, 2-ethyl-4-methylimidazole, methyl ethyl diketone network, zinc acetylacetonate, benzyl trimethyl ammonium chloride, trolamine borate, triethanol amine titanate, triphenylphosphine and salt, 1 thereof, 8-diaza-dicyclo (5,4,0) one or more of-7-undecylene and organic salt and 2-benzylimidazoline.
20. according to claim 11ly build composition, it is characterized in that described filler is selected from silica flour, aluminum oxide, aluminium hydroxide, magnesium hydroxide, barium sulfate, calcium carbonate, one or more of boron nitride and aluminium nitride.
21. according to claim 11ly build composition, it is characterized in that the median size of described filler is 1 μm ~ 50 μm.
22. according to building composition as cured article, for epoxy casting system one of claim 11 ~ 21 Suo Shu.
23. according to building composition as cured article for mesohigh electric installation mould material and electronic encapsulation material one of claim 11 ~ 21 Suo Shu.
Produce the described method of building composition of one of claim 11 ~ 21 for 24. 1 kinds, first produce the first component and the second composition respectively, then by the first component and second component mixing.
25. according to claim 24ly produce the method for building composition, it is characterized in that in temperature 70 C ~ 80 DEG C, stir 500r/min ~ 1500r/min and vacuum tightness 0.07MPa ~ 0.13MPa condition under, by weight, epoxy resin 20 ~ 50, ester cpds 5 ~ 30 and filler 30 ~ 80 are mixed, time 2 h ~ 3 hour, obtained the first described component.
26. according to claim 24ly produce the method for building composition, it is characterized in that under temperature 65 DEG C ~ 75 DEG C, stirring 500r/min ~ 1500r/min and vacuum tightness 0.07MPa ~ 0.13MPa condition, by weight, anhydride curing agent 15 ~ 45, curing catalyst 0.01 ~ 0.3 and filler 30 ~ 80 are mixed, time 2 h ~ 3 hour, obtained described second component.
27. according to claim 24ly produce the method for building composition, it is characterized in that in temperature 70 C ~ 80 DEG C, under stirring 500r/min ~ 1500r/min and vacuum tightness 0.07MPa ~ 0.13MPa condition, the first described component and described second component are mixed.
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| CN (1) | CN105566679A (en) |
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| CN105906814A (en) * | 2016-06-13 | 2016-08-31 | 四川大学 | Epoxy-terminated polyether and preparation method thereof and application thereof to serve as epoxy resin toughening agent |
| CN107573495A (en) * | 2017-09-20 | 2018-01-12 | 天守(福建)超纤科技股份有限公司 | A kind of flexible unsaturated polyester resin |
| CN111286289A (en) * | 2018-12-07 | 2020-06-16 | 浙江荣泰科技企业有限公司 | High-heat-conductivity adhesive |
| CN111825953A (en) * | 2020-07-16 | 2020-10-27 | 浙江荣泰科技企业有限公司 | Epoxy anhydride encapsulating composition and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105906814A (en) * | 2016-06-13 | 2016-08-31 | 四川大学 | Epoxy-terminated polyether and preparation method thereof and application thereof to serve as epoxy resin toughening agent |
| CN107573495A (en) * | 2017-09-20 | 2018-01-12 | 天守(福建)超纤科技股份有限公司 | A kind of flexible unsaturated polyester resin |
| CN111286289A (en) * | 2018-12-07 | 2020-06-16 | 浙江荣泰科技企业有限公司 | High-heat-conductivity adhesive |
| CN111825953A (en) * | 2020-07-16 | 2020-10-27 | 浙江荣泰科技企业有限公司 | Epoxy anhydride encapsulating composition and preparation method thereof |
| CN111825953B (en) * | 2020-07-16 | 2022-10-28 | 浙江荣泰科技企业有限公司 | Epoxy anhydride encapsulating composition and preparation method thereof |
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