CN103361019B - Epoxy resin pouring sealant - Google Patents
Epoxy resin pouring sealant Download PDFInfo
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- CN103361019B CN103361019B CN201310335976.XA CN201310335976A CN103361019B CN 103361019 B CN103361019 B CN 103361019B CN 201310335976 A CN201310335976 A CN 201310335976A CN 103361019 B CN103361019 B CN 103361019B
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Abstract
The invention discloses an epoxy resin pouring sealant. The epoxy resin pouring sealant comprises the component A--an epoxy resin and the component B--a curing agent. The component A comprises, by weight, 85 to 89% of a bisphenol A epoxy resin, 3 to 13% of a diluent and 0.15 to 0.25% of a defoaming agent. The component B comprises a first raw material and a second raw material, wherein the first raw material comprises, by weight, 40% of 1,3-BAC, 20% of the bisphenol A epoxy resin and 40% of benzyl alcohol, the second raw material comprises, by weight, 50% of isophorone diamine, 15% of the bisphenol A epoxy resin and 35% of benzyl alcohol, and the first raw material and the second raw material with same weight are mixed and stirred to obtain the component B. A weight ratio of the component A to the component B is 2: 1. The sum of the upper limit value of any component of the component A and the lower limit value of the rest components is no more than 100%, and the sum of the lower limit value of any component of the component A and the upper limit value of the rest components is no less than 100%. The epoxy resin pouring sealant provided by the invention has improved hardness, thermal deformation, voltage resistance, etc.
Description
Technical field
The present invention relates to a kind of epoxy resin embedding adhesive, particularly a kind of epoxy resin embedding adhesive for encapsulating the electron devices such as store battery.
Background technology
Epoxy resin is a kind of thermosetting resin, has excellent chemical stability, erosion resistance, and its adhesiveproperties is good, physical strength is high, electrical insulating property is strong, industrially be widely used, especially in the cast, encapsulation of the device such as electron device, transformer, be widely used especially.But, pure epoxy resin has high crosslinking structure, thus there is the shortcomings such as matter is crisp, fatiguability, thermotolerance are good not, toughness is poor, and epoxy resin embedding adhesive is epoxy resin and epoxy curing agent is obtained by mixing, which overcome above-mentioned shortcoming, more extensive in the practical application of electron device embedding, but there is the shortcomings such as hardness is low, thermal distortion is poor, withstand voltage properties is weak in existing epoxy resin embedding adhesive, needs to improve existing epoxy resin embedding adhesive.
Summary of the invention
For the problems referred to above that prior art exists, the invention provides a kind of epoxy resin embedding adhesive, by preparing epoxy resin and solidifying agent according to special process, be separated when not using and preserve, user mixes according to use step with certainweight ratio, stirs again in use, and then the epoxy resin embedding adhesive prepared all is improved in aspects such as serviceable time inherent hardness, thermal distortion and proof voltages.
A kind of epoxy resin embedding adhesive of the present invention, comprise the component A and B component that are separated and preserve, wherein component A is epoxy resin, component A comprises bisphenol A type epoxy resin, thinner and defoamer, calculate according to the weight ratio accounting for component A, bisphenol A type epoxy resin is 85%-89%, and thinner is 3%-13%, and defoamer is 0.15%-0.25%; B component is solidifying agent, B component comprises the first raw material and the second raw material, wherein the first raw material comprises 1,3-BAC (1,3-hexamethylene dimethylamine), bisphenol A type epoxy resin and phenylcarbinol, calculate according to part by weight, in the first raw material 1,3-BAC is 40%, and bisphenol A type epoxy resin is 20%, and phenylcarbinol is 40%; Second raw material comprises isophorone diamine, bisphenol A type epoxy resin and phenylcarbinol, and calculate according to part by weight, in the second raw material, isophorone diamine is 50%, and bisphenol A type epoxy resin is 15%, and phenylcarbinol is 35%; First raw material of identical weight and the second raw material mix and blend are obtained B component; In the part by weight of component A, lower value≤100% of higher limit+other formation components of arbitrary formation component of component A, higher limit >=100% of lower value+other formation components of arbitrary formation component of component A, when not using, component A is separated preservation with B component, when it is desired to be used component A and B component are mixed in container with the ratio of weight ratio 2: 1 under 25 DEG C of conditions and stir 2 minutes, until component A fully mixes with B component, obtain epoxy resin embedding adhesive.
Further, described thinner is reactive thinner.
Further, described reactive thinner is benzyl glycidyl ether and/or butylglycidyl ether, and benzyl glycidyl ether is 3%-7% at the part by weight of component A, and butylglycidyl ether is 3%-6% at the part by weight of component A.
Further, described defoamer is polysiloxane.
Further, when described component A only adds described bisphenol A type epoxy resin, preheating 30 minutes at 40 DEG C.
Further, after in component A, all formation component adds, mix and blend at constant temperature 60 DEG C.
Further, described component A also comprises the toner presenting color, makes the epoxy resin embedding adhesive produced present corresponding color.
Further, described toner comprises in white titanium dioxide, presents the red red powder be made up of gorgeous good scarlet pigment, presents the blue blue powder be made up of phthalocyanine blue pigment, and the part by weight that the gross weight of one or more toners described is shared in component A is 1%-2%.
Further, described B component is the first raw material and the second raw material mix and blend at constant temperature 80 DEG C.
Further, described epoxy resin embedding adhesive can use in 15-25 minute under 25 DEG C of conditions.
A preparation method for above-mentioned arbitrary described epoxy resin embedding adhesive, comprises the following steps:
(1) component A is prepared: calculate according to part by weight, the bisphenol A type epoxy resin preheating at 40 DEG C accounting for component A weight 85%-89% is added the reactor for the preparation of component A after 30 minutes, afterwards by one or both of the benzyl glycidyl ether of 3%-7% and the butylglycidyl ether of 3%-6%, and the defoamer of 0.15%-0.25% also adds reactor, and stir 30 minutes at reactor being placed in constant temperature 60 DEG C, stirring velocity is 24rpm (rev/min), afterwards by stand-by in component A container containing, wherein in the part by weight of component A, lower value≤100% of higher limit+other formation components of arbitrary formation component of component A, higher limit >=100% of lower value+other formation components of arbitrary formation component of component A,
(2) B component is prepared: B component comprises the first raw material and the second raw material, calculate according to part by weight, weight is accounted for 1 of the first raw material weight 40%, 3-BAC (1,3-hexamethylene dimethylamine), the bisphenol A type epoxy resin of 20% and 40% phenylcarbinol mixing in a kettle., stir 20 minutes under 25 DEG C of conditions, stirring velocity is 600-800rpm, obtain the first raw material, afterwards by stand-by in the first raw material container containing; In addition weight is accounted for the isophorone diamine of the second raw material weight 50%, the bisphenol A type epoxy resin of 15% and 35% phenylcarbinol mixing in a kettle., stir 20 minutes under 25 DEG C of conditions, stirring velocity is 600-800rpm, obtain the second raw material, afterwards by stand-by in second another container of raw material splendid attire; Then the first raw material and the second raw material are blended in the reactor of preparation B component by identical weight, and stir at reactor being placed in constant temperature 80 DEG C, stirring velocity is 24rpm, until the first raw material fully mixes with the second raw material, afterwards by stand-by in B component container containing;
(3) when not using, being separated and depositing component A and B component;
(4) epoxy resin embedding adhesive is prepared: when needs use epoxy resin embedding adhesive, the component A deposit separation and B component are mixed in container with the ratio of weight ratio 2: 1 and stir 2 minutes under 25 DEG C of conditions, until component A fully mixes with B component, the epoxy resin embedding adhesive obtained can use in 15-25 minute under 25 DEG C of conditions.
Before component A starts preparation, if the phenomenon if the materials such as the reactive thinner of one or both compositions of bisphenol A type epoxy resin, benzyl glycidyl ether and butylglycidyl ether, defoamer or toner make moist, can also before preparation component A, by drying material, i.e. micro-moisture that makes moist adding the various material of heat abstraction, certainly this step nonessential step.
A kind of epoxy resin embedding adhesive of the present invention, by preparing epoxy resin and solidifying agent according to special process, be separated when not using and preserve, user mixes according to use step with certainweight ratio, stirs again in use, and then the epoxy resin embedding adhesive prepared all is improved within the serviceable time in hardness, thermal distortion and proof voltage etc., wherein defoamer is for eliminating the bubble that may contain in preparation process, and to ensure quality product, defoamer can be polysiloxane.In addition, the present invention also can as required, in epoxy resin preparation process, add toner to obtain the epoxy resin embedding adhesive of color required for user, for in specific occasion in order to distinguish or to represent different implications, as represented positive pole with redness, blue represent negative pole etc.
Accompanying drawing explanation
Fig. 1 is the epoxy resin preparation flow figure of the embodiment of the present invention 1;
Fig. 2 is solidifying agent preparation flow figure of the present invention;
Fig. 3 is the preparation flow figure of epoxy resin embedding adhesive of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1
As shown in Figure 1, (KRX300 is product type to a kind of epoxy resin embedding adhesive KRX300A/B of the present invention, A represents component A epoxy resin, B represents B component solidifying agent), when preparing component A epoxy resin KRX300A, calculate according to the part by weight in component A, first get weight and account for the bisphenol A type epoxy resin of component A weight 88.8% (following percentage figures content if no special instructions, implication is identical all therewith), preheating 30 minutes at 40 DEG C, afterwards bisphenol A type epoxy resin is placed in the reactor for the preparation of component A, the reactive thinner that the benzyl glycidyl ether of 5% and the butylglycidyl ether of 4% form is added again in reactor, and add the defoamer of 0.2%, defoamer is for eliminating the bubble that may contain in preparation process, to ensure quality product, defoamer can be polysiloxane.Also according to user's needs, corresponding toner can be added, make it present corresponding color.In Fig. 1, also add the white powder of 0.9%, the red powder of 1.1%, to obtain red component A epoxy resin, and then make the epoxy resin embedding adhesive prepared also for red, the part by weight sum of each component part of above-mentioned component A epoxy resin is just in time 100%.
After each formation component of above-mentioned component A epoxy resin all adds reactor, at the temperature of 60 DEG C, with 24rpm (rev/min) stirred autoclave, churning time is 30 minutes, to make to stir, thus obtains component A epoxy resin.After stirring terminates, by component A epoxy resin splendid attire in container, and detect.
In detection, choose the sample of the component A epoxy resin in container, detect the indexs such as proportion, viscosity and flash point.As shown in table 1, detect KRX300A and KRX300B according to GB12007.5 and GB12007.4 respectively, the interval obtaining KRX300A proportion is 1.1-1.3g/cm
3, the interval of viscosity is 2.5-3.5 × 10
3cPS, the interval of flash point is for being greater than 195 DEG C.
As shown in Figure 2, when preparing B component solidifying agent, B component solidifying agent comprises the first raw material and the second raw material, calculate according to part by weight equally, first weight is accounted for 1 of the first raw material weight 40%, 3-BAC that is 1,3-hexamethylene dimethylamine (following percentage figures content if no special instructions, implication is identical all therewith), the bisphenol A type epoxy resin of 20% and 40% phenylcarbinol mixing in a kettle., stir 20 minutes under 25 DEG C of conditions, stirring velocity is 600-800rpm, obtains the first raw material, afterwards by stand-by in the first raw material container containing; In addition weight is accounted for the isophorone diamine of the second raw material weight 50% (following percentage figures content if no special instructions, implication is identical all therewith), the bisphenol A type epoxy resin of 15% and 35% phenylcarbinol mixing in a kettle., stir 20 minutes under 25 DEG C of conditions, stirring velocity is 600-800rpm, obtain the second raw material, afterwards by stand-by in second another container of raw material splendid attire; Then the first raw material and the second raw material are blended in the reactor of preparation B component by identical weight, and stir at reactor being placed in constant temperature 80 DEG C, stirring velocity is 24rpm, until the first raw material fully mixes with the second raw material, afterwards by B component container containing, and detect;
In detection, choose the sample of the B component solidifying agent in container, detect the indexs such as proportion, viscosity and flash point.As shown in table 1, detect KRX300A and KRX300B according to GB12007.5 and GB12007.4 respectively, the interval obtaining KRX300B proportion is 0.95-1.05g/cm
3, the interval of viscosity is 200-300CPS, and the interval of flash point is for being greater than 165 DEG C.
Wherein, component A epoxy resin and B component solidifying agent are separately preserved.In use, user prepares epoxy resin embedding adhesive more in accordance with the following steps: as shown in Figure 3, component A epoxy resin qualified for aforementioned detection and B component solidifying agent are mixed in container with the ratio of weight ratio 2: 1 under 25 DEG C of conditions and stir 2 minutes, until component A and B component fully mix obtain epoxy resin embedding adhesive, to get quality be the epoxy resin embedding adhesive KRX300A/B of 100g is sample, as shown in table 1, respectively according to GB2411-1980, GB1634-79 and GB1048-78 detects the shore hardness of epoxy resin embedding adhesive KRX300A/B, the indexs such as heat-drawn wire and electric property proof voltage.Detect in serviceable time of 15-25 minute under 25 DEG C of conditions of finding to prepare according to above-mentioned preparation method, the shore hardness interval of epoxy resin embedding adhesive KRX300A/B is 70 °-80 °, heat-drawn wire is interval for being more than or equal to 87 DEG C, and the interval of electric property proof voltage is 18-20Kv/mm.And in time under 25 DEG C of conditions after 25 minutes, indices all presents decline in various degree, be unsuitable for using.
Concrete examination criteria and the detected result of component A epoxy resin KRX300A, B component solidifying agent KRX300B and epoxy resin embedding adhesive KRX300A/B are as shown in table 1.
The Testing index interval of acceptance table of table 1KRX300A, KRX300B and KRX300A/B
If the phenomenon if the materials such as the reactive thinner of one or both compositions of bisphenol A type epoxy resin, benzyl glycidyl ether and butylglycidyl ether, defoamer or toner make moist, can also before preparation component A, by drying material, i.e. micro-moisture that makes moist adding the various material of heat abstraction, certainly this step nonessential step.
The present invention is available to user and separates the component A epoxy resin and B component solidifying agent preserved, by user when epoxy resin embedding adhesive need be used, independently according to the proportions of the weight ratio 2: 1 of component A epoxy resin and B component solidifying agent, stir, and use within the serviceable time, the serviceable time is in 15-25 minute under 25 DEG C of conditions.
Embodiment 2
With each formation component, stirring velocity, churning time, acid extraction, the various trace routine of embodiment 1, use step all identical, only concrete each form component concentration time different.When preparing component A epoxy resin, calculate according to the part by weight in component A, the weight of bisphenol A type epoxy resin accounts for 86.8% of component A weight (following percentage figures content if no special instructions, implication is identical all therewith), account for the benzyl glycidyl ether of component A weight 6% and the butylglycidyl ether composition reactive thinner of 5.05%, defoamer accounts for component A weight 0.15%, also add the white powder of 0.9%, the blue powder of 1.1%, the part by weight sum of each component part of above-mentioned component A epoxy resin is just in time 100%.
In the present embodiment, preparation method, respectively formation component and content, Heating temperature and the time of B component is all identical with B component in embodiment 1, has not just set forth at this.In addition, the test rating of component A and B component and the interval of acceptance of each test rating all in the same manner as in Example 1, its concrete Testing index and interval of acceptance also as shown in table 1.
The present invention proposes a kind of new epoxy resin embedding adhesive, by choosing each formation component and part by weight thereof, the setting of stirring velocity and churning time, the detection of various trace routine, and use step, obtain hardness high, thermal distortion is good, the epoxy resin embedding adhesive that withstand voltage properties is strong, meet the market requirement, and can adjust color, according to the needs of user, by adding toner in the preparation of component A epoxy resin, and then obtain the component A epoxy resin of corresponding color, thus obtain the epoxy resin embedding adhesive of required color, to play the effect distinguished or warn in the occasion of some such as store batteries etc.
A kind of epoxy resin embedding adhesive of the present invention is not limited to the above-mentioned embodiment listed.Person of ordinary skill in the field should know, and above description is only specific embodiments of the invention, and any pro forma change that the basis of the present invention's design is made the present invention or amendment are all in protection scope of the present invention.
Claims (3)
1. for an epoxy resin embedding adhesive for encasing electronic components, it is characterized in that, described epoxy resin embedding adhesive comprises the component A and B component that are separated and preserve, wherein:
Component A is epoxy resin, and component A comprises bisphenol A type epoxy resin, reactive thinner and polysiloxane defoamers, wherein calculate according to part by weight, bisphenol A type epoxy resin accounts for 85%-89%, and reactive thinner accounts for 3%-13%, and polysiloxane defoamers accounts for 0.15%-0.25%, and described reactive thinner is benzyl glycidyl ether and/or butylglycidyl ether, the preheating at 40 DEG C of described bisphenol A type epoxy resin is added the reactor for the preparation of component A after 30 minutes, be one or both of the butylglycidyl ether of 3%-6% by accounting for benzyl glycidyl ether that component A part by weight is 3%-7% and accounting for component A part by weight afterwards, and the polysiloxane defoamers of 0.15%-0.25% also adds reactor, and stir 30 minutes at reactor being placed in constant temperature 60 DEG C, stirring velocity is 24rpm, afterwards by stand-by in component A container containing, wherein in the part by weight of component A, lower value≤100% of higher limit+other formation components of arbitrary formation component of component A, higher limit >=100% of lower value+other formation components of arbitrary formation component of component A,
B component is solidifying agent, B component comprises the first raw material and the second raw material, wherein the first raw material comprises 1,3-BAC (1,3-hexamethylene dimethylamine), bisphenol A type epoxy resin and phenylcarbinol, calculate according to part by weight, in the first raw material 1,3-BAC accounts for 40%, and bisphenol A type epoxy resin accounts for 20%, and phenylcarbinol accounts for 40%; Second raw material comprises isophorone diamine, bisphenol A type epoxy resin and phenylcarbinol, and calculate according to part by weight, in the second raw material, isophorone diamine accounts for 50%, and bisphenol A type epoxy resin accounts for 15%, and phenylcarbinol accounts for 35%; First raw material of identical weight and the second raw material mix and blend are obtained B component; By described 1,3-BAC (1,3-hexamethylene dimethylamine), the bisphenol A type epoxy resin in described first raw material and the mixing of the phenylcarbinol in described first raw material in a kettle., stir 20 minutes under 25 DEG C of conditions, stirring velocity is 600-800rpm, obtain the first raw material, afterwards by stand-by in the first raw material container containing; In addition the phenylcarbinol of the bisphenol A type epoxy resin of isophorone diamine, described second raw material and described second raw material is mixed in a kettle., stir 20 minutes under 25 DEG C of conditions, stirring velocity is 600-800rpm, obtains the second raw material, afterwards by stand-by in second another container of raw material splendid attire; Then the first raw material and the second raw material are blended in the reactor of preparation B component by identical weight, and stir at reactor being placed in constant temperature 80 DEG C, stirring velocity is 24rpm, until the first raw material fully mixes with the second raw material, afterwards by stand-by in B component container containing;
When not using, component A is separated preservation with B component, when it is desired to be used component A and B component are mixed in container with the ratio of weight ratio 2: 1 under 25 DEG C of conditions and stir 2 minutes, until component A fully mixes with B component, obtain epoxy resin embedding adhesive.
2. epoxy resin embedding adhesive according to claim 1, is characterized in that, described component A also comprises the toner presenting color, makes the epoxy resin embedding adhesive produced present corresponding color.
3. epoxy resin embedding adhesive according to claim 2, it is characterized in that, described toner comprises in white titanium dioxide, presents the red red powder be made up of gorgeous good scarlet pigment, presents the blue blue powder be made up of phthalocyanine blue pigment, and the part by weight that the gross weight of one or more toners described is shared in component A is 1%-2%.
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| CN201310335976.XA CN103361019B (en) | 2013-08-05 | 2013-08-05 | Epoxy resin pouring sealant |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105820785A (en) * | 2016-04-26 | 2016-08-03 | 安徽康瑞鑫电子科技有限公司 | Special capping rubber for storage batteries |
| CN105802564A (en) * | 2016-04-26 | 2016-07-27 | 安徽康瑞鑫电子科技有限公司 | Special prime glue for storage battery |
| CN105838306A (en) * | 2016-04-26 | 2016-08-10 | 安徽康瑞鑫电子科技有限公司 | LED (light-emitting diode) packaging adhesive |
| CN105820784A (en) * | 2016-04-26 | 2016-08-03 | 安徽康瑞鑫电子科技有限公司 | Flame-retardant epoxy resin pouring sealant |
| CN106674893A (en) * | 2016-11-24 | 2017-05-17 | 广东天环创新科技股份有限公司 | Waterproof and anti-leakage modified epoxy grouting material for subway engineering and preparation method of waterproof and anti-leakage modified epoxy grouting material |
| CN111004558A (en) * | 2019-11-08 | 2020-04-14 | 肖松 | Perfusion fluid for oil type capacitor and preparation method thereof |
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| CN103172831A (en) * | 2013-03-26 | 2013-06-26 | 东莞市赛恩思实业有限公司 | Epoxy resin composition for luminous characters |
| CN103224611A (en) * | 2013-05-15 | 2013-07-31 | 程梦喜 | Modified alicyclic amine curing agent and preparation method thereof |
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| US8735512B2 (en) * | 2008-04-09 | 2014-05-27 | Air Products And Chemicals, Inc. | Curing agent for low temperature cure applications |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103172831A (en) * | 2013-03-26 | 2013-06-26 | 东莞市赛恩思实业有限公司 | Epoxy resin composition for luminous characters |
| CN103224611A (en) * | 2013-05-15 | 2013-07-31 | 程梦喜 | Modified alicyclic amine curing agent and preparation method thereof |
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Address after: 236500 Anhui Province Jieshou City Tian Ying Industrial Park Road 1, Anhui Kang Ruixin Electronic Technology Co. Ltd. Patentee after: Anhui Kangruixin Electronic Technology Co., Ltd. Address before: 236500 Anhui Province Jieshou City Tian Ying Industrial Park Shunda road Anhui Kang Ruixin Electronic Technology Co. Ltd. Patentee before: Anhui Kangruixin Electronic Technology Co., Ltd. |
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