CN112979923B - Tri-functionality epoxy compound containing triazine ring and preparation method thereof - Google Patents
Tri-functionality epoxy compound containing triazine ring and preparation method thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/32—Epoxy compounds containing three or more epoxy groups
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Abstract
The invention provides a triazine ring-containing tri-functionality epoxy compound and a preparation method thereof. The triazine ring-containing trifunctional epoxy compound is represented by the formula (I), wherein n is an integer of 1 to 6, such as 1,2,3,4,5, 6; r1、R2Independently selected from H or F. The epoxy compound provided by the invention can be used as epoxy resin of epoxy resin pouring sealant, the obtained epoxy resin pouring sealant has excellent comprehensive performance, very high mechanical strength performance, excellent dielectric property and low water absorption, can reach the V1 flame retardant grade of UL-94 under the condition of not adding a flame retardant, can reach the V0 grade by adopting the preferred technical scheme, is halogen-free and phosphorus-free epoxy resin pouring sealant, and can meet the environmental protection requirements of various requirements.
Description
Technical Field
The invention belongs to the field of organic compounds, and particularly relates to a triazine ring-containing tri-functionality epoxy compound and a preparation method thereof.
Background
Along with the progress of modern society science and technology, the application of electronic components is more and more extensive, and the demand volume is bigger and bigger. The encapsulating material for the electronic components plays an important role in the reliability and stability of the encapsulating material. The relatively many potting materials currently used include phenolic resins, epoxy resins, polyester resins and polyamides. The epoxy resin is a main product of the pouring sealant for the electronic components at present due to excellent mechanical property and chemical corrosion resistance. However, epoxy resins generally require the addition of flame retardants because of their poor flame retardancy. At present, along with the requirement of environmental protection, the non-halogenated flame retardant is in the trend, the WEEE instruction of European Union, namely the instruction of 'scrap electronic and electrical equipment', requires that the limited materials in the electronic and electrical equipment clearly show the non-halogenated property, the information industry of China has not been able to me 'pollution control and management measures of electronic information products', and also requires that the electronic information products reduce the content of toxic and harmful substances. The common flame retardant in epoxy encapsulating materials often contains bromine or Sb2O3The flame retardant system is a hot point of research under the trend that the environmental protection safety standard is increasingly strict, and the green, environmental protection and halogen-free epoxy packaging material is used. The requirement of the halogen-free flame retardant is that the content of bromine or chlorine is required to be less than 900ppm and the total content of bromine and chlorine is required to be less than 1500ppm according to the requirement of the regulation IEC 61249-2-21, and no regulation limits and requirements are made on fluorine element at present.
The halogen-free flame-retardant epoxy resin pouring sealant has the effective means at present that phosphorus flame retardants, especially some reactive phosphorus flame retardants such as DOPO modified flame retardants, are added, or DOPO is directly grafted on epoxy resin, and compared with the added flame retardants of physical blending, the chemical modified flame retardant mode has better compatibility among components and better performance of cured products after curing. The flame retardant hardly releases toxic gas under the conditions of combustion or high temperature, and is a new development trend of the conventional flame retardant. However, the phosphorus flame retardant is toxic and may leak from the waste, and potential safety hazards exist in the use and storage of the raw materials. Therefore, if the epoxy resin pouring sealant can be used on the basis of no halogen, phosphorus can be continuously removed, and meanwhile, the epoxy resin pouring sealant can achieve a good flame retardant effect and is a blank in the market. In the face of increasingly severe environmental protection pressure and increasingly strict standards for pouring sealant, research and development of the epoxy resin pouring sealant have important scientific research significance and commercial value.
Besides the requirement of flame retardance, the potting adhesive material of the electronic component is required to have low water absorption rate, otherwise, in a humid environment, the heat is high-temperature humid and hot weather in the south, and if the water absorption rate cannot reach the standard, the water vapor can corrode and damage the electronic component, so that the electronic component is seriously scrapped.
Therefore, the development of the epoxy resin pouring sealant which has excellent comprehensive performance and meets the current green and environment-friendly requirements has important significance.
Disclosure of Invention
In order to overcome the defects that the epoxy resin pouring sealant in the prior art cannot reach the standard in environmental protection and the comprehensive performance does not slowly meet the requirements, the invention provides a halogen-free phosphorus-free flame-retardant bisphenol epoxy resin pouring sealant and a preparation method thereof. The halogen-free phosphorus-free flame-retardant bisphenol epoxy resin pouring sealant mainly adopts bisphenol epoxy resin, a certain amount of trifunctional epoxy compound taking 1,3, 5-triazine as a mother core is additionally added, and epoxy resin compounded with bisphenol AF epoxy resin is taken as a base material of the pouring sealant, the obtained pouring sealant can reach the V1 flame-retardant grade of UL94 under the condition of not adding a flame retardant, and the preferable technical scheme can reach the V0 grade; meanwhile, due to the existence of the tri-functionality epoxy compound, the cross-linking density after curing is larger than that of the common bisphenol epoxy resin, but the toughness is not adversely affected, the mechanical property is excellent, and the high cross-linking density also ensures low water absorption. The halogen-free phosphorus-free flame-retardant bisphenol epoxy resin pouring sealant provided by the invention has excellent comprehensive performance, is green and environment-friendly, and is a novel epoxy resin pouring sealant for electronic components.
In order to solve the technical problems, the invention provides the following technical scheme:
a triazine ring-containing trifunctional epoxy compound has a structure shown in formula (I):
n in formula (I) is an integer of 1 to 6, such as 1,2,3,4,5, 6; r1、R2Independently selected from H or F.
Preferably, the compound of formula (I) is compound 3 of the following structure:
the invention also provides a halogen-free phosphorus-free flame-retardant bisphenol epoxy resin pouring sealant which comprises the following raw materials in parts by mass: 100 parts of epoxy resin, 100 parts of filler, 150 parts of curing agent, 3-7 parts of curing accelerator, 5-30 parts of reactive diluent, 5-15 parts of toughening agent and 1-3 parts of silane coupling agent; the epoxy resin comprises bisphenol A epoxy resin, bisphenol AF epoxy resin and a triazine ring-containing trifunctional epoxy compound shown in a formula (I):
n in formula (I) is an integer of 1 to 6, such as 1,2,3,4,5, 6; r1、R2Independently selected from H or F.
The tri-functional epoxy compound containing a triazine ring shown in the formula (I) can be used as a substitute for part of the epoxy resin in the epoxy potting adhesive, and therefore, can also be referred to as a tri-functional epoxy resin.
Further, the mass ratio of the bisphenol A type epoxy resin, the bisphenol AF type epoxy resin and the epoxy resin shown in the formula (I) is 6-11: 3-5: 2-3; preferably, the mass ratio of the bisphenol A type epoxy resin, the bisphenol AF type epoxy resin and the epoxy compound shown in the formula (I) is 8-10: 3-4: 2.5.
preferably, the compound of formula (I) is compound 3 of the structure, i.e. corresponding to n =2, R1，R2Are all H:
the synthetic route for compound 3 is as follows:
further, compound 3 is obtained by a preparation method comprising the following steps:
(1) preparing 1- (2-bromoethyl) -4-methoxybenzene into a Grignard reagent under the action of magnesium and iodine, and reacting the Grignard reagent with cyanuric chloride to obtain a compound 1;
(2) reacting the obtained compound 1, glacial acetic acid and hydrobromic acid at the temperature of 100-120 ℃ to obtain a compound 2;
(3) and reacting the obtained compound with epoxy chloropropane under the action of alkali to obtain a compound 3.
The preparation of the Grignard reagent in the step (1) is well known in the art, and is specifically obtained by reacting 1- (2-bromoethyl) -4-methoxybenzene, magnesium chips and iodine at 30-45 ℃ for 1-2 h. Reacting the obtained Grignard reagent with cyanuric chloride at 40-60 ℃ for 5-15h, quenching, and performing column chromatography separation and purification to obtain the compound 1. The reaction of step (1) is preferably carried out in anhydrous THF.
In the step (2), the ratio of the amount of the compound 1 to the amounts of the glacial acetic acid and the hydrobromic acid is not particularly limited, and the glacial acetic acid and the hydrobromic acid are used in excess, and in one embodiment of the present invention, the molar ratio of the compound 1 to the glacial acetic acid and the hydrobromic acid is 1: 2-4:5-8. The reaction time of the step (2) is 30-50 h.
In the step (3), the alkali is sodium hydroxide aqueous solution. The mol ratio of the compound 2 to the epichlorohydrin is 1: 10-20. The epoxy chloropropane is greatly excessive, which is favorable for the yield of the reaction.
The bisphenol a type epoxy resins are well known in the art, such as E20, E35, E42, E44. Bisphenol A epoxy resins having epoxy values of from 0.3 to 0.45 are preferred.
The bisphenol AF epoxy resin is prepared from hexafluorobisphenol A and epichlorohydrin under alkaline conditions, and the preparation of the epoxy resin is well known in the field. For example, refer to "preparation and properties of bisphenol AF type epoxy resin/cyanate ester copolymer" [ science and engineering of Polymer materials ], Vol.33, No. 12. Preferably, the reaction conditions are controlled so that the epoxy value of the bisphenol AF epoxy resin is 0.3 to 0.45.
The filler is selected from at least one of silicon micropowder, boron nitride, aluminum hydroxide and magnesium hydroxide, and the particle size is 3-10 mu m.
The curing agent is an acid anhydride curing agent, such as at least one of methyltetrahydrophthalic anhydride, liquid methylhexahydrophthalic anhydride, hexahydrophthalic anhydride, and methylnadic anhydride.
The curing accelerator is selected from imidazole accelerators, such as at least one of 2-methylimidazole, 2-ethylimidazole, 2-propylimidazole, 2-phenylimidazole, 1-benzyl-2-methylimidazole and 1-aminoethyl-2-methylimidazole. The reactive diluent is at least one selected from propylene oxide o-tolyl ether, o-tolyl glycidyl ether, hexanediol diglycidyl ether, polypropylene glycol diglycidyl ether, ethylene glycol diglycidyl ether or butanediol diglycidyl ether. The dosage of the reactive diluent is mainly used for adjusting the viscosity of the pouring sealant. The viscosity of the potting adhesive is required by the requirement of the reagent, and is not particularly limited.
The toughening agent is selected from polyether polyol and aromatic ester which are compounded according to the mass ratio of 2-4:1-1.5, and the aromatic ester is selected from at least one of dimethyl phthalate, diethyl phthalate, dibutyl phthalate and dioctyl phthalate; the polyether polyols have molecular weights of 4000-6000, such as VORANOL 4701.
The silane coupling agent is selected from aminosilane coupling agents, such as at least one of KH550, KH912 and KH 792.
Optionally, the bisphenol epoxy resin pouring sealant provided by the invention further comprises various auxiliaries, such as a dispersing agent, a leveling agent, a defoaming agent and an ultraviolet light absorber. The type and amount thereof is well known in the art. For example, the dispersant is selected from at least one of BYK-163 and AFCONA S527; the leveling agent is at least one selected from BYK-358N, BYK-333; the defoaming agent is selected from at least one of AFCONA 2045 and BYK 054; the ultraviolet light absorber is selected from the group consisting of Huann 326 and basf 5151.
In a preferred technical scheme of the invention, the halogen-free phosphorus-free flame-retardant bisphenol epoxy resin is encapsulated into a double component of a component A and a component B, wherein the component A comprises epoxy resin, a reactive diluent, a toughening agent and a silane coupling agent; the component B comprises a curing agent and a curing accelerator.
The invention also provides a preparation method of the halogen-free phosphorus-free flame-retardant bisphenol epoxy resin pouring sealant, which comprises the following steps: the epoxy resin is prepared by feeding epoxy resin, a compound shown as a formula (I), a reactive diluent, a toughening agent and a silane coupling agent according to a ratio, stirring at a high speed until the mixture is uniform, adding a curing agent and a curing accelerator, and stirring at 40-60 ℃ until the mixture is uniform.
In order to be convenient to use, the epoxy resin pouring sealant is generally prepared into two components of a component A and a component B, and comprises the following steps:
(1) preparation of component A: the epoxy resin, the reactive diluent, the toughening agent and the silane coupling agent are added according to the proportion and stirred at a high speed until the mixture is uniform, thus obtaining the epoxy resin;
(2) preparation of the component B: the curing agent and the curing accelerator are fed and then heated to 40-60 ℃ and stirred evenly to obtain the curing agent.
When in use, the mass ratio of the component A to the component B is 100:40-60 according to the mass ratio of the sum of the epoxy resin in the component A and the epoxy compound shown in the formula (I) to the mass of the curing agent in the component B.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, 1,3,5 triazine trifunctional epoxy resin (namely epoxy compound shown in formula (I), such as compound 3) is adopted as part of epoxy resin, and the epoxy resin is compounded with conventional bisphenol A epoxy resin and bisphenol AF epoxy resin with F atoms according to a certain proportion to obtain the epoxy resin pouring sealant, so that the epoxy resin pouring sealant has excellent comprehensive performance, very high mechanical strength performance, excellent dielectric property and low water absorption, can reach the V1 flame retardant level of UL-94 under the condition of not adding a flame retardant, can reach the V0 level by a preferred technical scheme, is a halogen-free and phosphorus-free epoxy resin pouring sealant, and can meet the environmental protection requirements of various requirements.
Detailed Description
Preparation example 1 preparation of Compound 3
(1) Adding 5mL of THF solution of 1- (2-bromoethyl) -4-methoxybenzene into a three-necked flask under the protection of nitrogen, adding newly-treated magnesium chips and small-particle iodine, heating and stirring, slowly dropping 0.1mol/L of THF solution of 1- (2-bromoethyl) -4-methoxybenzene after reaction initiation, and keeping the temperature under stirring for 40 DEG CoC, reacting for 1h to obtain a format reagent solution for later use.
Nitrogen protection 0-10oC, 0.1mol of cyanuric chloride is dissolved in dry THF, the Grignard reagent is dripped into the cyanuric chloride solution, and 40 percent of cyanuric chloride solution is dripped after the dripping is finishedoC, reacting for 10 hours, and quenching by using a saturated ammonium chloride solution. And performing column chromatography separation after extraction to obtain the compound 1.1 H NMR (300 MHz, CDCl3) 6.88-7.26 (12H, m), 3.75 (9H, s), 2.73 (6H,t), 2.40( 6H,t)。
(2) And adding 500mL of glacial acetic acid and 120mL of HBr into 50g of the compound 1, reacting at 110 ℃ for 48h, pouring into distilled water for precipitation, filtering, washing with deionized water, and drying in vacuum to obtain a compound 2.1 H NMR (300 MHz, CDCl3) 6.91-7.28 (12H, m),5.47(3H,s)，2.74 (6H，t),2.39(6H,t)
(3)0.1mol of compound 2 and 1mol of Epichlorohydrin (ECH) are mixed evenly, heated to 70 ℃, stirred and slowly heatedDropwise adding 30wt% NaOH aqueous solution, keeping the temperature at 70 ℃, continuing to react for 2h, adding deionized water, taking the organic phase, carrying out vacuum distillation to remove excessive epichlorohydrin, washing with water, and washing with alcohol to obtain a product compound 3.1 H NMR (300 MHz, CDCl3) 6.87-7.28 (12H, m), 4.21(6H, d) 3.57(t,3H), 2.72-2.76(12H, m), 2.41(6H, t). The infrared spectrum of the compound 3 was observed at 912-915 cm-1The characteristic absorption peak of epoxy group appears at 3100--1The characteristic peak of (a) substantially disappears, indicating that the phenolic hydroxyl group has been epoxidized. The epoxide number is tested to be 0.485 and the theoretical value is 0.492 by adopting a hydrochloric acid-acetone method.
Preparation example 2
And introducing nitrogen into the reaction vessel to remove air, refluxing 1mol of bisphenol AF and 10mol of epoxy chloropropane for 1h at 80 ℃ under the stirring condition in the presence of tetraethylammonium bromide, slowly dropwise adding a 30wt% NaOH aqueous solution, continuously refluxing and reacting for 4h at 80 ℃, removing the solvent under reduced pressure, cooling and filtering to obtain the bisphenol AF epoxy resin. The epoxy value was 0.41 by the hydrochloric acid-acetone method. Example 1
(1) Preparation of component A: adding 55.2 parts of bisphenol A epoxy resin E42, 27.6 parts of bisphenol AF epoxy resin (epoxy value is 0.41), 17.2 parts of compound 3, 120 parts of silicon powder, 20 parts of propylene oxide o-tolyl ether, 6 parts of VORANOL 4701 and 3 parts of diethyl phthalate into a high-speed stirrer, and uniformly stirring to obtain a component A;
(2) preparation of the component B: and (3) uniformly stirring 50 parts of isophorone diamine and 5 parts of 2-methylimidazole in a high-speed stirrer to obtain a component B.
Example 2
The other conditions and procedure were the same as in example 1 except that the epoxy resin in component A was 64.5 parts of bisphenol A epoxy resin E42, 19.4 parts of bisphenol AF epoxy resin and 16.1 parts of Compound 3.
Example 3
The other conditions and procedure were the same as in example 1 except that the epoxy resin in component A was 54.5 parts of bisphenol A epoxy resin E42, 27.3 parts of bisphenol AF epoxy resin and 18.2 parts of Compound 3.
Example 4
The other conditions and procedure were the same as in example 1 except that in the A component, the epoxy resin was 42.8 parts of bisphenol A epoxy resin E42, 35.7 parts of bisphenol AF epoxy resin, 21.5 parts of Compound 3.
Example 5
The other conditions and procedure were the same as in example 1 except that in the A component, the epoxy resin was 68.7 parts of bisphenol A epoxy resin E42, 18.7 parts of bisphenol AF epoxy resin, and 12.6 parts of Compound 3.
Example 6
The other conditions and procedure were the same as in example 1 except that in the A component, the epoxy resin was 57.9 parts of bisphenol A epoxy resin E42, 17.7 parts of bisphenol AF epoxy resin, and 17.7 parts of Compound 3.
Example 7
The other conditions and procedure were the same as in example 1 except that in the A component, the epoxy resin was 64.6 parts of bisphenol A epoxy resin E42, 26.3 parts of bisphenol AF epoxy resin, and 12.6 parts of Compound 3.
Example 8
The other conditions and procedure were the same as in example 1 except that in the A component, the epoxy resin was 61.5 parts of bisphenol A epoxy resin E42, 30.8 parts of bisphenol AF epoxy resin, and 7.7 parts of Compound 3.
Example 9
The other conditions and procedure were the same as in example 1 except that in the A component, the epoxy resin was 64 parts of bisphenol A epoxy resin E42, 16 parts of bisphenol AF epoxy resin, and 20 parts of Compound 3.
Example 10
The other conditions and procedure were the same as in example 1, except that in the preparation of component A, 9 parts of VORANOL 4701 was used as the toughening agent, i.e.diethyl phthalate was not added.
Example 11
The other conditions and procedure were the same as in example 1, except that in the preparation of component A, the toughening agent was 9 parts diethyl phthalate, i.e. no VORANOL 4701 was added.
Comparative example 1
The other conditions and procedure were the same as in example 1 except that in the A component, the epoxy resin was 66.7 parts of bisphenol A epoxy resin E42 and 33.3 parts of bisphenol AF epoxy resin, that is, compound 3 was not added.
Comparative example 2
The other conditions and procedure were the same as in example 1 except that in the A component, the epoxy resin was 76.2 parts of bisphenol A epoxy resin E42, and 23.8 parts of Compound 3, i.e., no bisphenol AF epoxy resin was added.
Application example
The mass ratio of the component A to the component B of the above examples and comparative examples is that the mass ratio of the epoxy resin in the component A to the curing agent in the component B is 100: 50, carrying out the feeding ratio of the component A and the component B, precuring the obtained pouring sealant for 2h at 100 ℃, and then carrying out hot press molding by using a hot press, wherein the hot press condition is 140 ℃/6MPa/6h, and the obtained substrate condensate is subjected to the following performance test, and the result is shown in Table 1:
the data in table 1 show that the halogen-free phosphorus-free flame-retardant bisphenol epoxy resin pouring sealant provided by the invention has excellent comprehensive performance, particularly can reach the V1 grade under the condition of not adding a flame retardant, and can reach the V0 grade in most embodiments. The data of comparative examples 1 and 2 show that the combination of bisphenol AF epoxy resin and compound 3 in the epoxy resin is crucial, and the flame retardant rating of V1 cannot be achieved. The synergistic cooperation of the F and the N elements of the two generates excellent flame retardant effect. In addition, the trifunctional compound 3 can enhance the crosslinking density of the cured product, and also has a beneficial effect on the low water absorption and mechanical strength of the cured product.
Claims (9)
1. A preparation method of a triazine ring-containing trifunctional epoxy compound 3 is characterized in that the synthetic route is as follows:
2. the process according to claim 1, wherein Compound 3 is obtained by a process comprising the steps of:
(1)1- (2-bromoethyl) -4-methoxybenzene is prepared into a Grignard reagent under the action of magnesium and iodine, and the Grignard reagent reacts with cyanuric chloride to obtain a compound 1;
(2) reacting the obtained compound 1, glacial acetic acid and hydrobromic acid at the temperature of 100-120 ℃ to obtain a compound 2;
(3) and reacting the obtained compound 2 with epoxy chloropropane under the action of alkali NaOH to obtain a compound 3.
3. The preparation method according to claim 2, wherein the grignard reagent in the step (1) is prepared by reacting 1- (2-bromoethyl) -4-methoxybenzene with magnesium chips and iodine at 30-45 ℃ for 1-2 h; reacting the Grignard reagent with cyanuric chloride at 40-60 ℃ for 5-15h, quenching, and performing column chromatography separation and purification to obtain a compound 1; in the step (2), the molar ratio of the compound 1 to the glacial acetic acid and the hydrobromic acid is 1: 2-4: 5-8; in the step (3), the alkali is sodium hydroxide aqueous solution, and the molar ratio of the compound 2 to the epichlorohydrin is 1: 10-20.
4. The halogen-free phosphorus-free flame-retardant bisphenol epoxy resin pouring sealant comprises the following raw materials in parts by mass: 100 parts of epoxy resin, 100 parts of filler, 150 parts of curing agent, 3-7 parts of curing accelerator, 5-30 parts of reactive diluent, 5-15 parts of toughening agent and 1-3 parts of silane coupling agent; the epoxy resin comprises bisphenol A epoxy resin, bisphenol AF epoxy resin and a triazine ring-containing trifunctional epoxy compound shown in a formula (I):
wherein n is an integer from 1 to 6; r1、R2Is H.
5. The epoxy resin potting adhesive of claim 4, wherein the triazine ring-containing trifunctional epoxy compound is compound 3:
6. the epoxy resin potting adhesive of claim 4, wherein the mass ratio of the bisphenol A type epoxy resin, the bisphenol AF type epoxy resin and the triazine ring-containing trifunctional epoxy compound is 6-11: 3-5: 2-3.
7. The epoxy potting adhesive of claim 4, wherein the bisphenol A epoxy resin is at least one selected from the group consisting of E20, E35, E42, E44; the filler is selected from at least one of silicon micropowder, boron nitride, aluminum hydroxide and magnesium hydroxide, and the particle size is 3-10 mu m; the curing agent is an anhydride curing agent; the curing accelerator is selected from imidazole accelerators; the reactive diluent is selected from at least one of o-tolyl glycidyl ether, hexanediol diglycidyl ether, polypropylene glycol diglycidyl ether, ethylene glycol diglycidyl ether or butanediol diglycidyl ether; the silane coupling agent is selected from aminosilane coupling agents.
8. The epoxy resin pouring sealant according to claim 4, wherein the toughening agent is selected from polyether polyol and aromatic ester in a mass ratio of 2-4:1-1.5, and the aromatic ester is selected from at least one of dimethyl phthalate, diethyl phthalate, dibutyl phthalate and dioctyl phthalate; the molecular weight of the polyether polyol is 4000-6000.
9. The method for preparing the epoxy resin pouring sealant of any one of claims 4 to 8, comprising the steps of: the epoxy resin, the filler, the reactive diluent, the toughening agent and the silane coupling agent are added according to the proportion, stirred at high speed until the mixture is uniform, then the curing agent and the curing accelerator are added, and the mixture is stirred at the temperature of 40-60 ℃ until the mixture is uniform, thus obtaining the epoxy resin-modified epoxy resin;
the two-component epoxy resin pouring sealant comprises the following steps:
(1) preparation of component A: the epoxy resin, the filler, the reactive diluent, the toughening agent and the silane coupling agent are added according to the proportion and stirred at a high speed until the mixture is uniform, thus obtaining the epoxy resin-modified epoxy resin;
(2) preparation of the component B: the curing agent and the curing accelerator are fed and then heated to 40-60 ℃ and stirred evenly to obtain the curing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110428458.7A CN112979923B (en) | 2021-04-21 | 2021-04-21 | Tri-functionality epoxy compound containing triazine ring and preparation method thereof |
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| US3053798A (en) * | 1959-04-22 | 1962-09-11 | Dal Mon Research Co | Polymerizable triazines and polymers thereof |
| JP3494256B2 (en) * | 1995-09-27 | 2004-02-09 | 日立化成工業株式会社 | Resin composition for water-based paint |
| CN102516914A (en) * | 2011-11-21 | 2012-06-27 | 烟台德邦电子材料有限公司 | Halogen-free flame-retardant epoxy resin electronic pouring sealant |
| CN104152093B (en) * | 2014-08-16 | 2016-04-27 | 烟台德邦科技有限公司 | A kind of flame-retarded heat-conducting double-component epoxy resin embedding adhesive and preparation method thereof |
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