CN103351580A - Preparation method of epoxy resin pouring sealant - Google Patents
Preparation method of epoxy resin pouring sealant Download PDFInfo
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- CN103351580A CN103351580A CN2013103359774A CN201310335977A CN103351580A CN 103351580 A CN103351580 A CN 103351580A CN 2013103359774 A CN2013103359774 A CN 2013103359774A CN 201310335977 A CN201310335977 A CN 201310335977A CN 103351580 A CN103351580 A CN 103351580A
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Abstract
The invention discloses a preparation method of an epoxy resin pouring sealant. The preparation method comprises the following steps of: (1) mixing and stirring 85%-89% of bisphenol A epoxy resin, 3%-13% of diluent and 0.15%-0.25% of defoamer together to obtain epoxy resin; (2) mixing and stirring 1,3-cyclohexyldimethylamine accounting for 40% of the weight of a first raw material, bisphenol A epoxy resin accounting for 20% of the weight of the first raw material and benzyl alcohol accounting for 40% of the weight of the first raw material together, thereby obtaining the first raw material, and mixing and stirring isophorone diamine accounting for 50% of the weight of a second raw material, bisphenol A epoxy resin accounting for 15% of the weight of the second raw material and benzyl alcohol accounting for 35% of the weight of the second raw material together, thereby obtaining the second raw material; then mixing and stirring the two raw materials together, thereby obtaining a curing agent; (3) when not in use, storing the epoxy resin and the curing agent separately; (4) when the epoxy resin sealant needs to be used, mixing and stirring the epoxy resin and curing agent together to obtain the epoxy resin pouring sealant. The epoxy resin pouring sealant prepared by the method provided by the invention is improved in al aspects of hardness, thermal deformation, voltage resistance and the like.
Description
Technical field
The present invention relates to a kind of preparation method of epoxy resin embedding adhesive, particularly a kind of preparation method of the epoxy resin embedding adhesive for electron device such as encapsulation store battery etc.
Background technology
Resins, epoxy is a kind of thermosetting resin, has good chemical stability, erosion resistance, and its adhesiveproperties is good, physical strength is high, electrical insulating property is strong, be widely used industrial, especially aspect the cast of the devices such as electron device, transformer, encapsulation, be widely used especially.But, pure epoxy resin has high crosslinking structure, thereby there are shortcomings such as matter is crisp, fatiguability, thermotolerance is good not, toughness is poor, mix with epoxy curing agent and get and epoxy resin embedding adhesive is Resins, epoxy, it has overcome above-mentioned shortcoming, more extensive in the practical application of electron device embedding, however there are the shortcomings such as hardness is low, thermal distortion is poor, withstand voltage properties is weak in existing epoxy resin embedding adhesive, need to improve existing epoxy resin embedding adhesive.
Summary of the invention
The problems referred to above for the prior art existence, the invention provides a kind of preparation method of epoxy resin embedding adhesive, by prepare Resins, epoxy and solidifying agent according to special process, when not using, separate and preserve, the user mixes, stirs with the certainweight ratio according to the use step more in use, and then the epoxy resin embedding adhesive of preparing all is improved in aspects such as inherent hardness of serviceable time, thermal distortion and proof voltages.
The preparation method of a kind of epoxy resin embedding adhesive of the present invention may further comprise the steps:
(1) preparation A component: wherein the A component is Resins, epoxy, calculate according to part by weight, the bisphenol A type epoxy resin of 85%-89% is added reactor for the preparation of the A component, afterwards the thinner of 3%-13% and the defoamer of 0.15%-0.25% are also added reactor, and with reactor stirring 30 minutes, stirring velocity is 24rpm (turning/per minute), afterwards with stand-by in the A component container containing, in the part by weight of A component, the lower value of the higher limit of arbitrary formation component of A component+other formation components≤100%, the higher limit of the lower value of arbitrary formation component of A component+other formation components 〉=100%;
(2) preparation B component: wherein the B component is solidifying agent, the 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%, and 3-BAC (1,3-hexamethylene dimethylamine), 20% bisphenol A type epoxy resin and 40% phenylcarbinol are blended in the reactor, under 25 ℃ of conditions, stirred 20 minutes, stirring velocity is 600-800rpm, obtains the first raw material, afterwards with stand-by in the first raw material container containing; The isophorone diamine, 15% bisphenol A type epoxy resin and 35% the phenylcarbinol that in addition weight are accounted for the second raw material weight 50% are blended in the reactor, under 25 ℃ of conditions, stirred 20 minutes, stirring velocity is 600-800rpm, obtain the second raw material, afterwards with 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, stirring velocity is 24rpm, until the first raw material and the second raw material fully mix, afterwards with stand-by in the B component container containing;
(3) when not using, separate and deposit A component and B component;
(4) preparation epoxy resin embedding adhesive: when needs use epoxy resin glue, the A component that separation is deposited and B component are mixed in the container with 2: 1 ratio of weight ratio under 25 ℃ of conditions and stirred 2 minutes, until A component and B component fully mix to obtain epoxy resin embedding adhesive.
Further, described bisphenol A type epoxy resin adds reactor for the preparation of the A component 40 ℃ of lower preheatings after 30 minutes.
Further, it is characterized in that, after described bisphenol A type epoxy resin, thinner and defoamer all add reactor, described reactor is placed 60 ℃ of lower stirrings of constant temperature.
Further, described the first raw material and described the second raw material are blended in the reactor of preparation B component by identical weight, and reactor is placed 80 ℃ of lower stirrings of constant temperature.
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 A component, and butylglycidyl ether is 3%-6% at the part by weight of A component.
Further, described defoamer is polysiloxane.
Further, described epoxy resin embedding adhesive uses in 15-25 minute under 25 ℃ of conditions.
Further, described A component also can comprise the toner that presents color, so that the epoxy resin embedding adhesive of producing presents corresponding color.
Further, described toner comprises the titanium dioxide that is white in color, present red powder that red gorgeous good scarlet pigment makes, present the blue blue powder of being made by phthalocyanine blue pigment, and the gross weight of described one or more toners shared part by weight in the A component is 1%-2%.
Before the A component begins 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 be before preparation A component, by the baking material, be little moisture that makes moist that adds the various materials of heat abstraction, certainly this step and nonessential step.
The preparation method of a kind of epoxy resin embedding adhesive of the present invention, by prepare Resins, epoxy and solidifying agent according to special process, when not using, separate and preserve, the user is again according to using step to mix, stir with the certainweight ratio in use, and then the epoxy resin embedding adhesive of preparing all was improved at aspects such as hardness, thermal distortion and proof voltages within the serviceable time, wherein defoamer is used for eliminating the bubble that preparation process may contain, to guarantee quality product, defoamer can be polysiloxane.In addition, the present invention also can be as required, in the Resins, epoxy preparation process, add toner to obtain the epoxy resin embedding adhesive of the required color of user, be used in the specific occasion in order to distinguish or to represent different implications, as representing positive pole with redness, blue expression negative pole etc.
Description of drawings
Fig. 1 is the Resins, epoxy preparation method's of the embodiment of the invention 1 schema;
Fig. 2 is solidifying agent preparation method's of the present invention schema;
Fig. 3 is epoxy resin embedding adhesive preparation method's of the present invention schema.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
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 the A component epoxy, B represents B component solidifying agent) the preparation method, when preparation A component epoxy KRX300A, calculate according to the part by weight in the A component, (following per-cent numeral content if no special instructions at first to get the bisphenol A type epoxy resin that part by weight accounts for A composition weight 88.8%, all implication is identical therewith), 40 ℃ of lower preheatings 30 minutes, afterwards bisphenol A type epoxy resin is placed the reactor for the preparation of the A component, add again the reactive thinner that the butylglycidyl ether of 5% benzyl glycidyl ether and 4% forms in the reactor, and add 0.2% defoamer, defoamer is used for eliminating the bubble that preparation process may contain, to guarantee quality product, defoamer can be polysiloxane.Also can add corresponding toner according to user's needs, make it present corresponding color.Among Fig. 1, also add 0.9% white powder, 1.1% red powder, obtaining red A component epoxy, and then so that the epoxy resin embedding adhesive of preparing also for red, the part by weight sum of each component part of above-mentioned A component epoxy just in time is 100%.
Behind respectively the consisting of component and all add reactor of above-mentioned A component epoxy, under 60 ℃ temperature, with 24rpm (rev/min) stirred autoclave, churning time is 30 minutes, so that stir, thereby obtains the A component epoxy.After stir finishing, A component epoxy splendid attire in container, and is detected.
In the detection, the A component epoxy of choosing in the container is sample, detects 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 that obtains 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 greater than 195 ℃.
As shown in Figure 2, when preparation 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, at first part by weight is accounted for 1 of the first raw material weight 40%, 3-BAC is 1, (following per-cent numeral content if no special instructions for 3-hexamethylene dimethylamine, all implication is identical therewith), 20% bisphenol A type epoxy resin and 40% phenylcarbinol be blended in the reactor, under 25 ℃ of conditions, stirred 20 minutes, stirring velocity is 600-800rpm, obtains the first raw material, afterwards with stand-by in the first raw material container containing; (following per-cent numeral content if no special instructions in addition part by weight to be accounted for the isophorone diamine of the second raw material weight 50%, all implication is identical therewith), 15% bisphenol A type epoxy resin and 35% phenylcarbinol be blended in the reactor, under 25 ℃ of conditions, stirred 20 minutes, stirring velocity is 600-800rpm, obtain the second raw material, afterwards with stand-by in second another container of raw material splendid attire; Then be blended in the first raw material and the second raw material in the reactor of preparation B component by identical weight, and reactor being placed 80 ℃ of constant temperature are lower to be stirred, stirring velocity is 24rpm, until the first raw material and the second raw material fully mix, afterwards with in the B component container containing, and detect;
In the detection, choose the sample of the B component solidifying agent in the 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 that obtains KRX300B proportion is 0.95-1.05g/cm
3, the interval of viscosity is 200-300CPS, the interval of flash point is greater than 165 ℃.
Wherein, A component epoxy and B component solidifying agent are separately preserved.In use, the user prepares epoxy resin embedding adhesive more in accordance with the following steps: as shown in Figure 3, the A component epoxy that aforementioned detection is qualified and B component solidifying agent are mixed in the container with 2: 1 ratio of weight ratio under 25 ℃ of conditions and stirred 2 minutes, until fully mixing, A component and B component obtain epoxy resin embedding adhesive, the epoxy resin embedding adhesive KRX300A/B that gets quality and be 100g is sample, as shown in table 1, respectively according to GB2411-1980, GB1634-79 and GB1048-78 detect the shore hardness of epoxy resin embedding adhesive KRX300A/B, the indexs such as heat-drawn wire and electric property proof voltage.Detect to find in 15-25 minute the serviceable time under 25 ℃ of conditions according to above-mentioned preparation method's preparation, the shore hardness interval of epoxy resin embedding adhesive KRX300A/B is 70 °-80 °, the heat-drawn wire interval is more than or equal to 87 ℃, and the interval of electric property proof voltage is 18-20Kv/mm.And under 25 ℃ of conditions in the time after 25 minutes, indices all presents decline in various degree, is unsuitable for using.
Concrete examination criteria and the detected result of A component epoxy KRX300A, B component solidifying agent KRX300B and epoxy resin embedding adhesive KRX300A/B are as shown in table 1.
The detection qualified interval table of table 1 KRX300A, 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 be before preparation A component, by the baking material, be little moisture that makes moist that adds the various materials of heat abstraction, certainly this step and nonessential step.
The present invention provides A component epoxy and the B component solidifying agent of separately preserving to the user, by the user when need use epoxy resin embedding adhesive, autonomous 2: 1 ratio proportioning of weight ratio according to A component epoxy and B component solidifying agent, stir, and within the serviceable time, use, the serviceable time is in 15-25 minute under 25 ℃ of conditions.
The present invention proposes a kind of preparation method of new epoxy resin embedding adhesive, by each formation component and part by weight thereof are chosen, the setting of stirring velocity and churning time, the detection of various trace routines, and use step, obtain the hardness height, thermal distortion is good, the epoxy resin embedding adhesive that withstand voltage properties is strong, satisfied the market requirement, and can adjust color, needs according to the user, by in the preparation of A component epoxy, adding toner, and then obtain the A component epoxy of corresponding color, thereby obtain the epoxy resin embedding adhesive of required color, distinguish or the effect of caution to play in some occasions such as store battery etc.
Embodiment 2
With respectively the consisting of component, stirring velocity, churning time, acid extraction, various trace routine, use step all identical, only different when specifically respectively consisting of component concentration of embodiment 1.When preparation A component epoxy, calculate according to the part by weight in the A component, the weight of bisphenol A type epoxy resin account for the A composition weight 86.8% (following per-cent numeral content if no special instructions, all implication is identical therewith), account for the benzyl glycidyl ether of A composition weight 6% and 5.05% butylglycidyl ether and form reactive thinner, defoamer accounts for A composition weight 0.15%, also add 0.9% white powder, 1.1% blue powder, the part by weight sum of each component part of above-mentioned A component epoxy just in time is 100%.
The preparation method of B component and epoxy resin embedding adhesive in the present embodiment, respectively consist of component and content thereof, Heating temperature and time respectively with embodiment 1 in B component and epoxy resin embedding adhesive identical, just do not set forth at this.In addition, the detection index of A component, B component and epoxy resin embedding adhesive and the detected result that respectively detects index all with embodiment 1 in identical, it specifically detects index and detected result is also as shown in table 1.
The preparation method of a kind of epoxy resin embedding adhesive of the present invention is not limited to the above-mentioned embodiment that lists.The person of ordinary skill in the field should know, and more than describing only is specific embodiments of the invention, and any pro forma change of on the basis of the present invention's design the present invention being made or modification are all in protection scope of the present invention.
Claims (10)
1. the preparation method of an epoxy resin embedding adhesive is characterized in that, may further comprise the steps:
(1) preparation A component: wherein the A component is Resins, epoxy, calculate according to the weight ratio that accounts for the A component, the bisphenol A type epoxy resin of 85%-89% is added reactor for the preparation of the A component, afterwards the thinner of 3%-13% and the defoamer of 0.15%-0.25% are also added reactor, and with reactor stirring 30 minutes, stirring velocity is 24rpm (turning/per minute), afterwards with stand-by in the A component container containing, in the part by weight of A component, the lower value of the higher limit of arbitrary formation component of A component+other formation components≤100%, the higher limit of the lower value of arbitrary formation component of A component+other formation components 〉=100%;
(2) preparation B component: wherein the B component is solidifying agent, the 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%, and 3-BAC (1,3-hexamethylene dimethylamine), 20% bisphenol A type epoxy resin and 40% phenylcarbinol are blended in the reactor, under 25 ℃ of conditions, stirred 20 minutes, stirring velocity is 600-800rpm, obtains the first raw material, afterwards with stand-by in the first raw material container containing; The isophorone diamine, 15% bisphenol A type epoxy resin and 35% the phenylcarbinol that in addition weight are accounted for the second raw material weight 50% are blended in the reactor, under 25 ℃ of conditions, stirred 20 minutes, stirring velocity is 600-800rpm, obtain the second raw material, afterwards with 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, stirring velocity is 24rpm, until the first raw material and the second raw material fully mix, afterwards with stand-by in the B component container containing;
(3) when not using, separate and deposit A component and B component;
(4) preparation epoxy resin embedding adhesive: when needs use epoxy resin glue, the A component that separation is deposited and B component are mixed in the container with 2: 1 ratio of weight ratio under 25 ℃ of conditions and stirred 2 minutes, until A component and B component fully mix to obtain epoxy resin embedding adhesive.
2. the preparation method of a kind of epoxy resin embedding adhesive according to claim 1 is characterized in that, described bisphenol A type epoxy resin adds reactor for the preparation of the A component 40 ℃ of lower preheatings after 30 minutes.
3. the preparation method of a kind of epoxy resin embedding adhesive according to claim 2 is characterized in that, after described bisphenol A type epoxy resin, thinner and defoamer all add reactor, described reactor is placed 60 ℃ of lower stirrings of constant temperature.
4. the preparation method of a kind of epoxy resin embedding adhesive according to claim 3 is characterized in that, described the first raw material and described the second raw material is blended in the reactor of preparation B component by identical weight, and reactor is placed 80 ℃ of lower stirrings of constant temperature.
5. the preparation method of a kind of epoxy resin embedding adhesive according to claim 4 is characterized in that, described thinner is reactive thinner.
6. the preparation method of a kind of epoxy resin embedding adhesive according to claim 5, it is characterized in that, described reactive thinner is benzyl glycidyl ether and/or butylglycidyl ether, benzyl glycidyl ether is 3%-7% at the part by weight of A component, and butylglycidyl ether is 3%-6% at the part by weight of A component.
7. the preparation method of a kind of epoxy resin embedding adhesive according to claim 6 is characterized in that, described defoamer is polysiloxane.
8. the preparation method of a kind of epoxy resin embedding adhesive according to claim 7 is characterized in that, described epoxy resin embedding adhesive uses in 15-25 minute under 25 ℃ of conditions.
9. the preparation method of the described a kind of epoxy resin embedding adhesive of any one is characterized in that according to claim 1-8, and described A component also can comprise the toner that presents color, so that the epoxy resin embedding adhesive of producing presents corresponding color.
10. the preparation method of a kind of epoxy resin embedding adhesive according to claim 9, it is characterized in that, described toner comprises the titanium dioxide that is white in color, present the red red powder of being made by gorgeous good scarlet pigment, present the blue blue powder of being made by phthalocyanine blue pigment, and the gross weight of described one or more toners shared part by weight in the A component is 1%-2%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1798249A1 (en) * | 2005-12-16 | 2007-06-20 | Mitsubishi Gas Chemical Company, Inc. | Curing agent composition for epoxy resins and epoxy resin composition |
| CN101735564A (en) * | 2009-12-22 | 2010-06-16 | 上海康达化工有限公司 | Vacuum infusion resin for wind turbine blades and preparation method thereof |
| 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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2013
- 2013-08-05 CN CN201310335977.4A patent/CN103351580B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1798249A1 (en) * | 2005-12-16 | 2007-06-20 | Mitsubishi Gas Chemical Company, Inc. | Curing agent composition for epoxy resins and epoxy resin composition |
| CN101735564A (en) * | 2009-12-22 | 2010-06-16 | 上海康达化工有限公司 | Vacuum infusion resin for wind turbine blades and preparation method thereof |
| 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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