CN104044231A - Non post cure epoxy resin casting system - Google Patents
Non post cure epoxy resin casting system Download PDFInfo
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- CN104044231A CN104044231A CN201410202861.8A CN201410202861A CN104044231A CN 104044231 A CN104044231 A CN 104044231A CN 201410202861 A CN201410202861 A CN 201410202861A CN 104044231 A CN104044231 A CN 104044231A
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Abstract
The invention provides a non post cure epoxy resin casting system including a formula toughening epoxy resin and a formula toughening anhydride curing agent; the formula toughening epoxy resin is milk white to pale yellow solvent-free pre-acceleration liquid epoxy resin; the formula toughening anhydride curing agent is an improved pre-acceleration anhydride liquid curing agent; components are mixed at the lower temperature in the desired quantity, are defoamed under vacuum condition for 0.5 to 2 hours after even mixing, and then are poured into a mold for curing reaction. The non post cure epoxy resin casting system has the following main characteristics: after demoulding, curing is not needed, the comprehensive energy consumption of electrical equipment manufacturing plants can be reduced, the production cycle time can be shortened by more than 20%, the product delivery time can be shortened, the product cost and labor intensity of workers can be reduced.
Description
Technical field
The present invention relates to epoxy resin casting system, particularly reach the non-rear cured epoxy resin casting system of one that needs the rear equal electromechanical properties of cured epoxy system without rear solidifying.
Background technology
Epoxy resin has good physical and mechanical property, electrical insulation capability, chemical resistance and adhesive property, can be used as coating, casting material, molding compound, adhesive, laminated material with the form that directly or indirectly uses the various aspects for the national economy from daily living article to high-technology field.Especially in electric insulation field, epoxy resin occupies very important status, but at present the production technology of main flow adopts two kinds of traditional vacuum pouring and automatic pressure gels (APG), and the common feature of these two kinds of techniques is exactly all after the goods demoulding, again under approximately 130 celsius temperatures, to reach the rear solidification process of 10 hours.After this, solidification process is to eliminate the internal stress at inner accumulation in first paragraph solidification process, and to not having completely crued part again to solidify.But this traditional curing process also can bring the energy consumption of great number and heavier labour intensity, also affect the delivery date of product simultaneously.Therefore, study and develop a kind of non-rear cured epoxy resin casting system and curing thereof very necessary.
Summary of the invention
In order to overcome the above-mentioned shortcoming of prior art, to the object of this invention is to provide, shortened up to 20% the production cycle of equipment manufacturers, reduce the energy resource consumption of factory and alleviate the non-rear cured epoxy resin casting system of one of workman's labour intensity.
The technical solution adopted for the present invention to solve the technical problems is: a kind of non-rear cured epoxy resin casting system, comprise epoxy resin toughened, the toughness reinforcing anhydride curing agent of filling a prescription of formula, wherein: described formula is epoxy resin toughened is that milky is to light yellow solvent-free preaceleration liquid epoxies, the toughness reinforcing anhydride curing agent of described formula is improvement preaceleration acid anhydrides liquid curing-agent, and described formula production technology epoxy resin toughened and the toughness reinforcing anhydride curing agent of formula is as follows:
1) fill a prescription epoxy resin toughened: at 25 DEG C-200 DEG C, the flexibilizer of 1%-40% ratio is added in epoxy resin, keep thermotonus 1-5 hour, question response finishes to be cooled to normal temperature, adds 0.001%-0.5% promoter to stir 30-120 minute, filters and packages;
2) the toughness reinforcing anhydride curing agent of filling a prescription: at 25 DEG C-200 DEG C, the flexibilizer of 1%-40% ratio and 0.001%-0.3% catalyst are added in acid anhydrides, keep thermotonus 1-5 hour, question response finishes to be cooled to 25 DEG C-150 DEG C, add 0.05%-5% promoter to stir 30-120 minute, cooled and filtered packaging;
Be 25 DEG C-80 DEG C to mix according to 1:1:3-4 ratio in temperature by epoxy resin toughened formula, the active silica flour of fill a prescription toughness reinforcing anhydride curing agent and 400 orders, mix, under vacuum condition, carry out pouring into mould after vacuum defoamation 0.5-2 hour and be cured reaction, curing reaction finishes the rear demoulding and obtains product, solidifies without rear.
As a further improvement on the present invention: described flexibilizer includes but not limited to polyol, epoxidation or non-epoxidized vegetable oil, thermoplastic, reactivity or non-reactive liquid rubber, single two or many epoxy radicals glycidol ether, long chain alkylphenol, containing functional group's long-chain diamine and binary acid, epoxy resin prepared by polyol or aliphatic acid, end is the mylar of hydroxyl or carboxyl, polyamide, end is the acrylonitrile-butadiene rubber of hydroxyl, polysulfide rubber.
As a further improvement on the present invention: described promoter includes but not limited to tertiary amine and salt, acetyl acetone salt, imidazoles and homologue, triphenylphosphine Ji Qi phosphonium salt, organic carboxylate.
As a further improvement on the present invention: described formula is epoxy resin toughened is extremely light yellow solvent-free preaceleration liquid epoxies of milky, and product data are:
Color: milky is to light yellow;
Viscosity at 25 DEG C: 2000-80000 mPa.s;
Viscosity at 60 DEG C: 120-1800 mPa.s;
Epoxy content: 4.50-5.50 eq/kg;
Density at 25 DEG C: 1.12-1.2 g/cm3;
Flash-point: 130-140 DEG C;
25 DEG C of vapour pressures: 0.01-0.02Pa.
As a further improvement on the present invention: the toughness reinforcing anhydride curing agent of described formula is improvement preaceleration acid anhydrides liquid curing-agent, and product data are:
Color: milky is to light yellow;
Viscosity at 25 DEG C: 3000-3500 mPa.s;
At 25 DEG C of lower density: 1.13-1.2;
Flash-point: 135-145 DEG C;
Vapour pressure at 25 DEG C: 0.5-15Pa.
Compared with prior art, the invention has the beneficial effects as follows:
1. in epoxy resin and curing agent, select appropriate efficient flexibilizer to reduce the cracking behaviors that in solidification process without issue, stress causes simultaneously.
2. in epoxy resin and curing agent, select appropriate promoter to promote the curing rate of non-rear cured epoxy resin casting system, to ensure that in first paragraph solidification process, non-rear cured epoxy resin casting system is completely curing.
By control different types of flexibilizer with and ratio deal with the toughening effect of different product.
By control different types of promoter with and ratio adjust the state of cure in first paragraph hardening time under uniform temperature and certain hour.
5. production technology is simple, and raw material sources are abundant, and production efficiency is high, and technological process is easily controlled.Thereby ensure the quality stability of product.
6. the product of preparation is added to non-metallic fillers and can produce non-rear cured epoxy cast product by traditional vacuum pouring or automatic pressure gel (APG).
7. the present invention exempts solidification process after epoxy-resin systems, is that epoxy product manufacturer reduces energy consumption.And shorten up to more than 20% time production cycle, shorten due date, reduce product cost and alleviate workman's labour intensity.The present invention has very large effect to the production environment of improving company with the economic benefit of the company of lifting.
Brief description of the drawings
The DSC table of the non-rear cured epoxy cast product of Fig. 1.
Detailed description of the invention
Now the present invention is further described in conjunction with the embodiments:
A kind of non-rear cured epoxy resin casting system, comprise epoxy resin toughened, the toughness reinforcing anhydride curing agent of filling a prescription of formula, wherein: described formula is epoxy resin toughened is that milky is to light yellow solvent-free preaceleration liquid epoxies, the toughness reinforcing anhydride curing agent of described formula is improvement preaceleration acid anhydrides liquid curing-agent, and described formula production technology epoxy resin toughened and the toughness reinforcing anhydride curing agent of formula is as follows:
1) fill a prescription epoxy resin toughened: at 25 DEG C-200 DEG C, the flexibilizer of 1%-40% ratio is added in epoxy resin, keep thermotonus 1-5 hour, question response finishes to be cooled to normal temperature, adds 0.001%-0.5% promoter to stir 30-120 minute, filters and packages;
2) the toughness reinforcing anhydride curing agent of filling a prescription: at 25 DEG C-200 DEG C, the flexibilizer of 1%-40% ratio and 0.001%-0.3% catalyst are added in acid anhydrides, keep thermotonus 1-5 hour, question response finishes to be cooled to 25 DEG C-150 DEG C, add 0.05%-5% promoter to stir 30-120 minute, cooled and filtered packaging.
Described flexibilizer Main Function is in order to alleviate the sharply cracking phenomena in dispose procedure of stress in solidification process without issue.
Described promoter Main Function is in order to accelerate solidifying of cured epoxy resin casting system without issue.
Be 25 DEG C-80 DEG C to mix according to 1:1:3-4 ratio in temperature by epoxy resin toughened formula, the active silica flour of fill a prescription toughness reinforcing anhydride curing agent and 400 orders, mix, under vacuum condition, carry out pouring into mould after vacuum defoamation 0.5-2 hour and be cured reaction, curing reaction finishes the rear demoulding and obtains product, solidifies without rear.
Described non-rear cured epoxy resin casting system is added to the non-metallic fillers of some, can prepare non-rear cured epoxy resin casting product.
Described formula is epoxy resin toughened is extremely light yellow solvent-free preaceleration liquid epoxies of milky, and product data are:
Color: milky is to light yellow
Viscosity at 25 DEG C: 2000-80000 mPa.s;
Viscosity at 60 DEG C: 120-1800 mPa.s;
Epoxy content: 4.50-5.50 eq/kg;
Density at 25 DEG C: 1.12-1.2 g/cm3;
Flash-point: 130-140 DEG C;
25 DEG C of vapour pressures: 0.01-0.02Pa;
The toughness reinforcing anhydride curing agent of described formula is improvement preaceleration acid anhydrides liquid curing-agent, and product data are:
Color: milky is to light yellow;
Viscosity at 25 DEG C: 3000-3500 mPa.s;
25 DEG C of lower densities: 1.13-1.2 g/cm3;
Flash-point: 135-145 DEG C;
Vapour pressure at 25 DEG C: 0.5-15Pa;
Acrylonitrile-butadiene rubber, polysulfide rubber that the epoxy resin that described flexibilizer includes but not limited to polyol, epoxidation or non-epoxidized vegetable oil, thermoplastic, reactivity or non-reactive liquid rubber, single two or many epoxy radicals glycidol ether, long chain alkylphenol, prepare containing functional group's long-chain diamine and binary acid, polyol or aliphatic acid, mylar, polyamide, the end that end is hydroxyl or carboxyl are hydroxyl.
Described promoter includes but not limited to tertiary amine and salt, acetyl acetone salt, imidazoles and homologue, triphenylphosphine Ji Qi phosphonium salt, organic carboxylate.
The present invention coordinates the nonmetal raw materials such as appropriate silica flour, manufactures transformer, the electric products such as insulator according to traditional vacuum cast or automatic pressure gel (APG).
In the present invention without the criterion of rear curing performance:
1. the glass transition temperature of differential scanning calorimetry (DSC) test solidfied material and solidifying without male offspring and the comparison of rear curing DSC curve.
Completion of cure: have obvious glass transition temperature and non-rear curing DSC curve there is no obvious exothermic peak in some high-temperature regions.
Solidify not exclusively: without obvious glass transition temperature, and there is obvious exothermic peak the non-rear curing some high-temperature regions of DSC curve.
2. test products cold cycling number of times in cold cycling baking oven, so that test products cracking performance.
Case study on implementation one:
At normal temperatures, by 10% LLQ8040,0.5% K560 and 0.5% DY062 promoter join in 89% DER331, and stir about 80 minutes, stand-by at normal temperatures.Under 80 degree by 0.8%DCMU-99 N-(3,4 dichlorophenyls)-N, N-dimethyl urea is dissolved in LLQ1225, is cooled to normal temperature stand-by.Then epoxy resin toughened above-mentioned formula, the active silica flour of fill a prescription toughness reinforcing anhydride curing agent and 400 orders are mixed 1 hour according to 100:100:380 at 40 DEG C, vacuumize 1.5 hours, 150 DEG C of mold temperatures, vacuum 4.5mbar, 160 DEG C of pressurizes 15 minutes, the demoulding draws an insulator, need not after solidify.DSC curve tested glass transition temperature is at 85 DEG C, and there is no above obvious exotherm at 100 DEG C.-40 DEG C of-80 DEG C of cold cycling 3 times are without any cracking phenomena.
Case study on implementation two:
By 5%ATBN 1300 × 21,0.2% K560 and 0.8% DMP30 promoter join in 94% DER331, and stir about 80 minutes, stand-by at normal temperatures.At 150 DEG C, by the methyl tetrahydro phthalic anhydride reaction of 10% Macrogol 200 and 89.5% 1.5 hours, be cooled to normal temperature to add 0.5%2-ethyl-4 methylimidazole, stir 30 minutes, be cooled to normal temperature stand-by.Then epoxy resin toughened above-mentioned formula, the active silica flour of fill a prescription toughness reinforcing anhydride curing agent and 400 orders are mixed 1 hour according to 100:100:350 at 40 DEG C, vacuumize 1.5 hours, 150 DEG C of mold temperatures, vacuum 4.5mbar, 150 DEG C of pressurizes 30 minutes, the demoulding draws a transformer, need not after solidify.DSC curve tested glass transition temperature is at 82 DEG C, and there is no above obvious exotherm at 100 DEG C.-50 DEG C of-120 DEG C of cold cycling 5 times are without any cracking phenomena.
Upper table is the cold cycling report of the non-rear cured epoxy cast product of production in case study on implementation two, and the conclusion of report is without any cracking phenomena.
Case study on implementation three:
At 80 DEG C, 0.2% aluminium acetylacetonate promoter is joined in 89.3% DER331 and dissolved, be then cooled to normal temperature, by 15%PPGDGE, 0.5% K560 adds in said mixture, stirs 1 hour, stand-by.Under 80 degree, 0.5% organic urea diphenylguanidine yhard UR 500 is dissolved in LLQ 1227, is cooled to normal temperature stand-by.Then epoxy resin toughened above-mentioned formula, the active silica flour of fill a prescription toughness reinforcing anhydride curing agent and 400 orders are mixed 1 hour according to 100:100:400 at 40 DEG C, vacuumize 1.5 hours, 150 DEG C of mold temperatures, vacuum 4.5mbar, 150 DEG C of pressurizes 20 minutes, the demoulding draws a sleeve pipe, need not after solidify.DSC curve tested glass transition temperature is about 96 DEG C, and there is no above obvious exotherm at 100 DEG C.-40 DEG C of-80 DEG C of cold cycling 3 times are without any cracking phenomena.
with reference to figure 1,the DSC table of the non-rear cured epoxy cast product of producing in case study on implementation three, as can be seen from the table, the epoxy casting goods that the present invention obtains do not have rear solidifying to approach complete solid state.
In sum, those of ordinary skill in the art reads after file of the present invention, makes other various corresponding conversion scheme according to technical scheme of the present invention and technical conceive without creative mental labour, all belongs to the scope that the present invention protects.
Claims (5)
1. a non-rear cured epoxy resin casting system, comprise epoxy resin toughened, the toughness reinforcing anhydride curing agent of filling a prescription of formula, it is characterized in that: described formula is epoxy resin toughened for milky is to light yellow solvent-free preaceleration liquid epoxies, the toughness reinforcing anhydride curing agent of described formula is improvement preaceleration acid anhydrides liquid curing-agent, and described formula production technology epoxy resin toughened and the toughness reinforcing anhydride curing agent of formula is as follows:
1) fill a prescription epoxy resin toughened: at 25 DEG C-200 DEG C, the flexibilizer of 1%-40% ratio is added in epoxy resin, keep thermotonus 1-5 hour, question response finishes to be cooled to normal temperature, adds 0.001%-0.5% promoter to stir 30-120 minute, filters and packages;
2) the toughness reinforcing anhydride curing agent of filling a prescription: at 25 DEG C-200 DEG C, the flexibilizer of 1%-40% ratio and 0.001%-0.3% catalyst are added in acid anhydrides, keep thermotonus 1-5 hour, question response finishes to be cooled to 25 DEG C-150 DEG C, add 0.05%-5% promoter to stir 30-120 minute, cooled and filtered packaging;
Be 25 DEG C-80 DEG C to mix according to 1:1:3-4 ratio in temperature by epoxy resin toughened formula, the active silica flour of fill a prescription toughness reinforcing anhydride curing agent and 400 orders, mix, under vacuum condition, carry out pouring into mould after vacuum defoamation 0.5-2 hour and be cured reaction, curing reaction finishes the rear demoulding and obtains product, solidifies without rear.
2. the non-rear cured epoxy resin casting system of one according to claim 1, is characterized in that: acrylonitrile-butadiene rubber, polysulfide rubber that the epoxy resin that described flexibilizer includes but not limited to polyol, epoxidation or non-epoxidized vegetable oil, thermoplastic, reactivity or non-reactive liquid rubber, single two or many epoxy radicals glycidol ether, long chain alkylphenol, prepare containing functional group's long-chain diamine and binary acid, polyol or aliphatic acid, mylar, polyamide, the end that end is hydroxyl or carboxyl are hydroxyl.
3. the non-rear cured epoxy resin casting system of one according to claim 1, is characterized in that: described promoter includes but not limited to tertiary amine and salt, acetyl acetone salt, imidazoles and homologue, triphenylphosphine Ji Qi phosphonium salt, organic carboxylate.
4. the non-rear cured epoxy resin casting system of one according to claim 1, is characterized in that: described formula is epoxy resin toughened for milky is to light yellow solvent-free preaceleration liquid epoxies, and product data are:
Color: milky is to light yellow;
Viscosity at 25 DEG C: 2000-80000 mPa.s;
Viscosity at 60 DEG C: 120-1800 mPa.s;
Epoxy content: 4.50-5.50 eq/kg;
Density at 25 DEG C: 1.12-1.2 g/cm3;
Flash-point: 130-140 DEG C;
25 DEG C of vapour pressures: 0.01-0.02Pa.
5. the non-rear cured epoxy resin casting system of one according to claim 1, is characterized in that: the toughness reinforcing anhydride curing agent of described formula is improvement preaceleration acid anhydrides liquid curing-agent, and product data are:
Color: milky is to light yellow;
Viscosity at 25 DEG C: 3000-3500 mPa.s;
At 25 DEG C of lower density: 1.13-1.2;
Flash-point: 135-145 DEG C;
Vapour pressure at 25 DEG C: 0.5-15Pa.
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| CN201410202861.8A CN104044231B (en) | 2014-05-14 | 2014-05-14 | A kind of non-post cured epoxy resin casting system |
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| CN201410202861.8A CN104044231B (en) | 2014-05-14 | 2014-05-14 | A kind of non-post cured epoxy resin casting system |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105061725A (en) * | 2015-08-12 | 2015-11-18 | 中国科学院兰州化学物理研究所 | Heat-resistant and high-toughness bisphenol A epoxy resin |
| CN105385109A (en) * | 2015-12-23 | 2016-03-09 | 宁波康伯斯电器有限公司 | Epoxy resin composition and application of epoxy resin composition in dipping coil preparation |
| CN105566679A (en) * | 2015-12-29 | 2016-05-11 | 浙江荣泰科技企业有限公司 | Ester compound, and preparation method and application thereof to epoxy resin casting system |
| CN106866936A (en) * | 2017-02-13 | 2017-06-20 | 广州仑利奇合成树脂有限公司 | A kind of bio-based electric insulation epoxy systems and preparation method thereof |
| CN107298754A (en) * | 2017-06-26 | 2017-10-27 | 广州仑利奇合成树脂有限公司 | A kind of many condensing models of liquid, its preparation method and application |
| CN107602887A (en) * | 2017-09-21 | 2018-01-19 | 上海稳优实业有限公司 | Exempt from the preparation method of the electric epoxy resin of solidify afterwards |
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| CN103086630A (en) * | 2013-02-01 | 2013-05-08 | 中铁大桥(郑州)缆索有限公司 | Chill casting filling for bridge cable chill casting anchorage and preparation method thereof |
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| CN102086365A (en) * | 2010-12-27 | 2011-06-08 | 东莞市腾威电子材料技术有限公司 | Adhesive, preparation method and application in integrated circuit board embedment thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105061725A (en) * | 2015-08-12 | 2015-11-18 | 中国科学院兰州化学物理研究所 | Heat-resistant and high-toughness bisphenol A epoxy resin |
| CN105385109A (en) * | 2015-12-23 | 2016-03-09 | 宁波康伯斯电器有限公司 | Epoxy resin composition and application of epoxy resin composition in dipping coil preparation |
| CN105566679A (en) * | 2015-12-29 | 2016-05-11 | 浙江荣泰科技企业有限公司 | Ester compound, and preparation method and application thereof to epoxy resin casting system |
| CN106866936A (en) * | 2017-02-13 | 2017-06-20 | 广州仑利奇合成树脂有限公司 | A kind of bio-based electric insulation epoxy systems and preparation method thereof |
| CN106866936B (en) * | 2017-02-13 | 2019-05-14 | 广州仑利奇合成树脂有限公司 | A kind of biology base electric insulation epoxy systems and preparation method thereof |
| CN107298754A (en) * | 2017-06-26 | 2017-10-27 | 广州仑利奇合成树脂有限公司 | A kind of many condensing models of liquid, its preparation method and application |
| CN107298754B (en) * | 2017-06-26 | 2019-06-28 | 广州仑利奇合成树脂有限公司 | A kind of liquid poly acid anhydrides, preparation method and application |
| CN107602887A (en) * | 2017-09-21 | 2018-01-19 | 上海稳优实业有限公司 | Exempt from the preparation method of the electric epoxy resin of solidify afterwards |
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| CN104044231B (en) | 2016-09-07 |
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