CN105131252A - Method for producing liquid-state epoxy resin through one step - Google Patents
Method for producing liquid-state epoxy resin through one step Download PDFInfo
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- CN105131252A CN105131252A CN201510656216.8A CN201510656216A CN105131252A CN 105131252 A CN105131252 A CN 105131252A CN 201510656216 A CN201510656216 A CN 201510656216A CN 105131252 A CN105131252 A CN 105131252A
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Abstract
The invention provides a method for producing liquid-state epoxy resin through one step. An epoxy resin solution obtained through a reaction is conveniently separated from saline water, subsequent separation is convenient, and low-cost intermediate products can be provided for solid-state epoxy resin production. The method includes the steps that A, by weight, 50-100 parts of bisphenol A and 100-150 parts of epoxy chloropropane are put into a reaction kettle, and heating and dissolving are conducted; B, the temperature is raised to 68-72 DEG C, an ring-opening etherification reaction is conducted, and then a sodium hydroxide solution with the concentration of 25% to 45% is added, and a cyclization chain propagation reaction is conducted; C, 50-80 parts of organic solvent is added for extraction after the reaction ends; D, the liquid-state epoxy resin is obtained after water washing, filtering and solvent separation are conducted.
Description
Technical field
The present invention relates to epoxy resin production method, be specifically related to a kind of production method of liquid-state 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.
For reaching the object of producing solid epoxy resin, must first production high-performance liquid-state epoxy resin.
Summary of the invention
Technical problem to be solved by this invention is a kind of method providing One-step production liquid-state epoxy resin, reaction gained epoxy resin solution, and with salt solution convenient separation, later separation is convenient, can produce provide low cost intermediate product for solid epoxy resin.
For solving the problems of the technologies described above, the method for One-step production liquid-state epoxy resin of the present invention, 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.
By weight, in described steps A, dihydroxyphenyl propane is 60 parts, and epoxy chloropropane is 120 parts; In described step B, hydrogen-oxygen is preferred, in described step C, uses toluene or methyl iso-butyl ketone (MIBK) as solvent.
Preferably, in described step C, use toluene as solvent.
Changing sodium solution is 26.5 parts, and its concentration is 30%; In described step C, organic solvent is 70 parts.
The technological merit of above step is embodied in: 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.
Use the liquid-state epoxy resin prepared by the present invention, can prepare solid epoxy resin further, concrete steps are as follows:
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.
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.
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
The present invention first prepares low molecular weight liquid epoxy, in subsequent technique, the low molecular weight liquid epoxy of preparation and dihydroxyphenyl propane can be used 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 (4)
1. the method for One-step production liquid-state 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.
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 C, uses toluene or methyl iso-butyl ketone (MIBK) as solvent.
4. 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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| Application Number | Priority Date | Filing Date | Title |
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| CN201510656216.8A CN105131252A (en) | 2015-10-12 | 2015-10-12 | Method for producing liquid-state epoxy resin through one step |
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| CN201510656216.8A CN105131252A (en) | 2015-10-12 | 2015-10-12 | Method for producing liquid-state epoxy resin through one step |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117511A (en) * | 2016-06-29 | 2016-11-16 | 黄山锦峰实业有限公司 | The production technology of epoxy resin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4132718A (en) * | 1975-12-19 | 1979-01-02 | Societa' Italiana Resine S.I.R. S.P.A. | Preparation of liquid epoxy resins from bisphenols |
| CN101613458A (en) * | 2008-06-25 | 2009-12-30 | 中国石油化工集团公司 | A kind of preparation method of bisphenol-A liquid epoxy resin |
-
2015
- 2015-10-12 CN CN201510656216.8A patent/CN105131252A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4132718A (en) * | 1975-12-19 | 1979-01-02 | Societa' Italiana Resine S.I.R. S.P.A. | Preparation of liquid epoxy resins from bisphenols |
| CN101613458A (en) * | 2008-06-25 | 2009-12-30 | 中国石油化工集团公司 | A kind of preparation method of bisphenol-A liquid epoxy resin |
Non-Patent Citations (2)
| Title |
|---|
| 李娟: "双酚A环氧树脂的合成及特种环氧树脂的固化行为与性能的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 杨东洁: "双酚A低分子环氧树脂的合成工艺研究", 《四川师范大学学报（自然科学版）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117511A (en) * | 2016-06-29 | 2016-11-16 | 黄山锦峰实业有限公司 | The production technology of epoxy resin |
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Application publication date: 20151209 |