CN105153402A - Method for producing electronic-grade epoxy resin through two-step method - Google Patents
Method for producing electronic-grade epoxy resin through two-step method Download PDFInfo
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- CN105153402A CN105153402A CN201510655449.6A CN201510655449A CN105153402A CN 105153402 A CN105153402 A CN 105153402A CN 201510655449 A CN201510655449 A CN 201510655449A CN 105153402 A CN105153402 A CN 105153402A
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Abstract
The invention provides a method for producing electronic-grade epoxy resin through a two-step method. The method comprises the following steps: A, taking and putting 50-100 parts by weight of bisphenol A and 100-150 parts by weight of epichlorohydrin into a reaction kettle, and heating for dissolving; B, heating to 68-72 DEG C, carrying out ring-opening etherification reaction, and adding a sodium hydroxide solution with the concentration of 25-45% of for cyclization chain growth reaction; C, adding 50-80 parts of an organic solvent for extracting; D, washing with water, filtering, and removing the solvent so as to obtain liquid epoxy resin; E, taking 320 parts of liquid epoxy resin obtained in the step D, heating to 90 DEG C, adding 280 parts of bisphenol A, and heating to 120 DEG C; F, adding 4 parts of an auxiliary, 5 parts of a reducing agent and 3 parts of an antioxidant, continuously heating to 170 DEG C, and carrying out heat preservation for 3 h; G, detecting whether the product is qualified or not, so as to obtain the solid epoxy resin after acceptance. The epoxy resin is short in production period, low in cost, stable in quality and less in side effects and a good environmental protection characteristic is realized in the production process.
Description
Technical field
The present invention relates to epoxy resin production method, be specifically related to a kind of production method of electronic-grade epoxy resin.
Background technology
The suitability for industrialized production of solid epoxy starts from the end of the fifties in last century in China, afterwards along with the development of society, production capacity and kind are also constantly in expansion, 1,800,000 present t/a are developed into by less than 1.5 ten thousand t/a, being widely used in environmental protection industry---the epoxy resin of the solid bisphenol A type of powder coating industry, also by 21.12 ten thousand ts of zero starting by 2010, is indispensable some in national economy.
Electric is the most important Application Areas of epoxy resin, and it is mainly used as the base material of copper-clad plate (CCL), is almost present in each electronic product.In prior art, the production technique of epoxy resin mainly contains method WATER-WASHING METHOD, catalysis-solvent method, two step body addition polymerization methods etc.Wherein, WATER-WASHING METHOD quality product is stable not, and the production cycle is long; The catalysis-solvent method production cycle is longer, and two step body addition polymerization method side reactions are many, and have branched structure in resultant, oxirane value is on the low side, and easily cause solidifying pot phenomenon during poorly soluble even reaction, large-scale production need not.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of two-step approach to produce the method for electronic-grade epoxy resin, and it is with short production cycle, cost is low, constant product quality, and side reaction is few, and production process environmental protection characteristic is good.
For solving the problems of the technologies described above, two-step approach of the present invention produces the method for electronic-grade epoxy resin, comprises the following steps:
A, by weight, get dihydroxyphenyl propane 50 ~ 100 parts, epoxy chloropropane 100 ~ 150 parts of input reactors, heating for dissolving;
B, be warming up to 68 ~ 72 DEG C and carry out ring opening etherification reaction, then add concentration be 25% ~ 45% sodium hydroxide solution carry out cyclisation transfer reaction;
C, reaction add 50 ~ 80 parts of organic solvents again after terminating and extract;
D, process washing, filtration, obtain liquid-state epoxy resin after desolventizing.
E, get step D gained liquid-state epoxy resin 320 parts and be warming up to 90 DEG C, add dihydroxyphenyl propane 280 parts, continue to be warming up to 120 DEG C;
F, add auxiliary agent 4 parts, reductive agent 5 parts, 3 parts, oxidation inhibitor, continue to be warming up to 170 DEG C, insulation 3h;
After G, sampling, detection are qualified finished solid epoxy resin.
By weight, in described steps A, dihydroxyphenyl propane is 60 parts, and epoxy chloropropane is 120 parts; In described step B, sodium hydroxide solution is 26.5 parts, and its concentration is 30%; In described step C, organic solvent is 70 parts.
Preferably, in described step F, auxiliary agent refers to that the trade mark that Kent, Zhejiang Province company of Chemical Co., Ltd. produces is B080 quaternary alkylphosphonium salt product, reductive agent refers to that the Shanghai Wei Fang Fine Chemical Co., Ltd trade mark is the product of Triphenylphospine oxide, and oxidation inhibitor refers to that Kent, the Zhejiang Province Chemical Co., Ltd. trade mark is the product of B150 trityl group phosphorus chloride.
Preferably, in described step C, use toluene or methyl iso-butyl ketone (MIBK) as solvent.
Preferably, in described step C, use toluene as solvent.
Technique scheme produces electronic-grade epoxy resin with two-step approach, and it is with short production cycle, cost is low, constant product quality, and side reaction is few, and production process environmental protection characteristic is good.
Embodiment
Two-step approach of the present invention produces the method for electronic-grade epoxy resin, first prepare low molecular weight liquid epoxy, again using low molecular weight liquid epoxy and dihydroxyphenyl propane as raw material, under catalyst action, obtain intermediate molecular weight solid epoxy by addition reaction.
Embodiment one
First with one-step synthesis method liquid epoxies, reaction formula is as follows:
A, get dihydroxyphenyl propane 6 tons, epoxy chloropropane 12 tons of input reactors, heating for dissolving;
B, be warming up to 70 ± 2 DEG C and carry out ring opening etherification reaction, then add concentration be 30% sodium hydroxide solution 2.65 tons carry out cyclisation transfer reaction;
C, reaction add 7 tons of toluene again after terminating and extract as organic solvent;
D, process washing, filtration, obtain liquid-state epoxy resin after desolventizing.
Above-mentioned steps A-D can prepare liquid epoxies, its process characteristic: the epoxy resin solution be 1. obtained by reacting, and with salt solution convenient separation, it is few that washing removes a small amount of NaCl hourly water consumption; 2. brine concentration is high, and it is low that multiple-effect evaporation reclaims salt energy consumption; 3. temperature of reaction is easy to control, and product color is shallow, transparency is high, mechanical impurity is few; 4. methyl iso-butyl ketone (MIBK) (MIBK) or toluene can be used as solvent, especially use toluene as solvent, can significantly reduce costs.
Table 1 embodiment one product performance synopsis
Embodiment two
The present embodiment for raw material, prepares electronic-grade solid epoxy resin with embodiment one gained liquid-state epoxy resin further.Comprise the following steps:
E, get step D gained liquid-state epoxy resin 320kg and be warming up to 90 DEG C, add dihydroxyphenyl propane 280kg, continue to be warming up to 120 DEG C;
F, add auxiliary agent 4kg, reductive agent 5kg, oxidation inhibitor 3kg, continue to be warming up to 170 DEG C, insulation 3h;
After G, sampling, detection are qualified finished solid epoxy resin.
Table 1 embodiment two product performance synopsis
The process characteristic of step e-G: 1. reaction is carried out in homogeneous phase, transfer reaction is comparatively steady, and obtained resin relative molecular mass distribution is narrower, and content of organic chloride is lower; 2. have that technique is simple, easy to operate, equipment is few, reaction time is short, reaction is thermopositive reaction, the heat release that reaction process can make full use of reaction maintains the energy needed for reacting, and energy consumption is low, by the solid epoxy regulating raw-material proportioning can produce Multiple Type.3. reaction is polyaddition reaction, and not having by product to produce, stopped the generation of " three wastes " from source, is green process for cleanly preparing.
Step e-G reaction formula is as follows:
In described step F, auxiliary agent refers to that the trade mark that Kent, Zhejiang Province company of Chemical Co., Ltd. produces is B080 quaternary alkylphosphonium salt product, reductive agent refers to that the Shanghai Wei Fang Fine Chemical Co., Ltd trade mark is the product of Triphenylphospine oxide, and oxidation inhibitor refers to that Kent, the Zhejiang Province Chemical Co., Ltd. trade mark is the product of B150 trityl group phosphorus chloride.
Table 3 solid epoxy production technique compares
Technical scheme of the present invention, first prepare lower molecular weight liquid-state epoxy resin, this product can directly use with single product; Invention further provides with this liquid-state epoxy resin for the production method of solid epoxy resin prepared by raw material, prepared product can be used for electric field and other field.
Claims (5)
1. two-step approach produces the method for electronic-grade epoxy resin, comprises the following steps:
A, by weight, get dihydroxyphenyl propane 50 ~ 100 parts, epoxy chloropropane 100 ~ 150 parts of input reactors, heating for dissolving;
B, be warming up to 68 ~ 72 DEG C and carry out ring opening etherification reaction, then add concentration be 25% ~ 45% sodium hydroxide solution carry out cyclisation transfer reaction;
C, reaction add 50 ~ 80 parts of organic solvents again after terminating and extract;
D, process washing, filtration, obtain liquid-state epoxy resin after desolventizing;
E, get step D gained liquid-state epoxy resin 320 parts and be warming up to 90 DEG C, add dihydroxyphenyl propane 280 parts, continue to be warming up to 120 DEG C;
F, add auxiliary agent 4 parts, reductive agent 5 parts, 3 parts, oxidation inhibitor, continue to be warming up to 170 DEG C, insulation 3h;
After G, sampling, detection are qualified finished solid epoxy resin.
2. two-step approach as claimed in claim 1 produces the method for electronic-grade epoxy resin, and it is characterized in that: by weight, in described steps A, dihydroxyphenyl propane is 60 parts, and epoxy chloropropane is 120 parts; In described step B, sodium hydroxide solution is 26.5 parts, and its concentration is 30%; In described step C, organic solvent is 70 parts.
3. two-step approach as claimed in claim 1 or 2 produces the method for electronic-grade epoxy resin, it is characterized in that, in described step F, auxiliary agent refers to that the trade mark that Kent, Zhejiang Province company of Chemical Co., Ltd. produces is B080 quaternary alkylphosphonium salt product, reductive agent refers to that the Shanghai Wei Fang Fine Chemical Co., Ltd trade mark is the product of Triphenylphospine oxide, and oxidation inhibitor refers to that Kent, the Zhejiang Province Chemical Co., Ltd. trade mark is the product of B150 trityl group phosphorus chloride.
4. two-step approach as claimed in claim 1 or 2 produces the method for electronic-grade epoxy resin, it is characterized in that, in described step C, uses toluene or methyl iso-butyl ketone (MIBK) as solvent.
5. two-step approach as claimed in claim 3 produces the method for electronic-grade epoxy resin, it is characterized in that, in described step C, uses toluene as solvent.
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| CN201510655449.6A CN105153402A (en) | 2015-10-12 | 2015-10-12 | Method for producing electronic-grade epoxy resin through two-step method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109749055A (en) * | 2018-12-27 | 2019-05-14 | 昆山市淀山湖宝波树脂涂料厂 | A kind of production technology of epoxy resin |
| CN112694718A (en) * | 2020-12-02 | 2021-04-23 | 江西戈兰帝电气绝缘材料有限公司 | Preparation method of epoxy resin electronic and electric insulating material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199275A (en) * | 2011-03-31 | 2011-09-28 | 安徽恒远化工有限公司 | Production technology for one-step synthesis of solid epoxy resin |
| CN103923299A (en) * | 2014-04-15 | 2014-07-16 | 江苏扬农锦湖化工有限公司 | Hard resin production technology |
| CN104130379A (en) * | 2014-07-22 | 2014-11-05 | 建滔(番禺南沙)石化有限公司 | Bisphenol A epoxy resin preparation method and product prepared therethrough |
-
2015
- 2015-10-12 CN CN201510655449.6A patent/CN105153402A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199275A (en) * | 2011-03-31 | 2011-09-28 | 安徽恒远化工有限公司 | Production technology for one-step synthesis of solid epoxy resin |
| CN103923299A (en) * | 2014-04-15 | 2014-07-16 | 江苏扬农锦湖化工有限公司 | Hard resin production technology |
| CN104130379A (en) * | 2014-07-22 | 2014-11-05 | 建滔(番禺南沙)石化有限公司 | Bisphenol A epoxy resin preparation method and product prepared therethrough |
Non-Patent Citations (1)
| Title |
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| 刘守贵: "固体双酚A型环氧树脂合成工艺述评", 《绝缘材料通讯》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109749055A (en) * | 2018-12-27 | 2019-05-14 | 昆山市淀山湖宝波树脂涂料厂 | A kind of production technology of epoxy resin |
| CN112694718A (en) * | 2020-12-02 | 2021-04-23 | 江西戈兰帝电气绝缘材料有限公司 | Preparation method of epoxy resin electronic and electric insulating material |
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Application publication date: 20151216 |