CN104725598A - Method for preparing modified epoxy resin - Google Patents
Method for preparing modified epoxy resin Download PDFInfo
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- CN104725598A CN104725598A CN201510142293.1A CN201510142293A CN104725598A CN 104725598 A CN104725598 A CN 104725598A CN 201510142293 A CN201510142293 A CN 201510142293A CN 104725598 A CN104725598 A CN 104725598A
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- epoxy resin
- cardanol
- anacardol
- bisphenol
- mol ratio
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Abstract
The invention discloses a method for preparing modified epoxy resin. The method comprises the following steps: weighing anacardol and bisphenol A, wherein the mol ratio of anacardol to bisphenol A is 1:1-10, adding anacardol and bisphenol A into a reaction container, and adding concentrated sulfuric acid into the reaction container, wherein the mass of concentrated sulfuric acid is 1-7% of that of anacardol; synthesizing an intermediate under the catalysis of concentrated sulfuric acid, adding epoxy chloropropane to the intermediate, wherein the mol ratio of the intermediate to the epoxy chloropropane is 1:1-10, and the temperature is 60-70 DEG C; dipping a sodium hydroxide solution, wherein the mol ratio of the intermediate to the sodium hydroxide solution is 1:1-10, after finishing dipping, keeping the temperature, reacting for 2-4h, rinsing, extracting, dewatering and weighing raw materials to obtain the anacardol modified bisphenol A epoxy resin. By adopting the method to modify the bisphenol A by the pure plant anacardol and synthesize the epoxy resin, the toughness of the epoxy resin is good, the heat resistance is increased, the resin viscosity is reduced and the modified epoxy resin is resistant to low-temperature curing.
Description
Technical field:
The invention belongs to chemical field, particularly relate to a kind of epoxy resin, specifically a kind of method preparing modified epoxy.
Background technology:
Petroleum engineering Institute for Research and Technology " development of modified by cardanol epoxy resin " adopts cashew shell liquid to be main raw material, at 250 DEG C, its cut and phenol reactant is got under the vacuum of 5 ~ 10mmHg, synthetic intermediate DNP, DNP becomes modified by cardanol epoxy resin entirely with epichlorohydrin reaction again, this resin flexible toughness supply exceed demand bisphenol A type epoxy resin, and Corrosion Protection is preeminent excellent, is a kind of desirable protection against corrosion base-material.
Shengyi Science and Technology Co., Ltd, Guangdong's " applied research of modified by cardanol epoxy resin " mainly have studied the addition (0-40wt%) of different modified by cardanol epoxy resin (CNSL-EP) to the impact by phenolic resin curing brominated bisphenol A epoxy resin (BPA-EP) system performance.Find through research, along with the increase of CNSL-EP addition, significantly declining has appearred in the stripping strength of Copper Foil, second-order transition temperature.CNSL-EP/BPA-EP co-mixing system mechanical property keeps better, and when CNSL-EP/BPA-EP weight ratio is 80/20, its cured article tensile strength, flexural strength, tensile modulus, modulus in flexure conservation rate are higher.Find that CNSL-EP Different adding amount does not have an impact to system 5% thermal weight loss temperature simultaneously.Adding of CNSL-EP can promote water-intake rate and dielectric properties to a certain extent.
Summary of the invention:
The object of the present invention is to provide a kind of method preparing modified epoxy, the described this method preparing modified epoxy solves epoxy resin toughness of the prior art, thermotolerance, low-temperature curing, technical problem that viscosity is larger.
The invention provides a kind of method preparing modified epoxy, first take cardanol and dihydroxyphenyl propane, described cardanol and the mol ratio of bis-phenol are 1:1 ~ 10, then above-mentioned cardanol and dihydroxyphenyl propane are joined in a reaction vessel, the vitriol oil is added again in described reaction vessel, the quality of the described vitriol oil is 1 ~ 7% of cardanol quality, described cardanol and dihydroxyphenyl propane synthesize intermediate under the catalysis of the vitriol oil, in intermediate, add epoxy chlorine compare alkane, described intermediate and epoxy chlorine are 1:1 ~ 10 than the mol ratio of alkane, temperature of reaction is 60 ~ 70 DEG C, drip sodium hydroxide solution again, described intermediate and sodium hydroxide mol ratio are 1:1 ~ 10, dropwise rear insulation 70 ~ 85 DEG C, react 2 ~ 4 hours, through washing, extraction, the epoxy resin of modified by cardanol dihydroxyphenyl propane is obtained after removing water and excess raw material.
The above-mentioned reaction process preparing the method for modified epoxy is as follows:
Further, the mass percent concentration of the described vitriol oil is 80 ~ 95%.
Further, the mass fraction of described sodium hydroxide is 30 ~ 50%.
The present invention utilizes a kind of pure plant modified by cardanol dihydroxyphenyl propane resynthesis epoxy resin, and make the toughness of epoxy resin better, thermotolerance increases, and resin viscosity decreases, more low temperature resistant solidification, improves the shortcoming of traditional dihydroxyphenyl propane solidifying agent to a great extent.
The present invention considers that the Long carbon chain of cardanol has good snappiness and can be used for modified bisphenol A type epoxy resin, the cardanol containing Long carbon chain structure is just connected before the non-synthesizing epoxy of dihydroxyphenyl propane, and then epoxidation obtains epoxy resin, make the toughness of epoxy resin better, thermotolerance increases, resin viscosity decreases, more low temperature resistant solidification.
The present invention compares with prior art, and its effect is actively with obvious.Modified by the present invention, make the toughness of epoxy resin better, thermotolerance increases, and resin viscosity decreases, more low temperature resistant solidification.
Embodiment:
Embodiment 1:
Cardanol 300 grams mixes through heating with dihydroxyphenyl propane 228 grams, under 5 grams of concentrated sulfuric acid catalyst effects, 100 DEG C are reacted 2 hours, synthesize intermediate, add epoxy chlorine again and maintain the temperature at 60 ~ 70 DEG C than 277.5 grams, alkane, drip the sodium hydroxide solution 100 grams of 30 ~ 50% mass fractions, be incubated to 80 degree of reactions 3 hours, through washing, extraction, removes water and excessive response raw material obtains target product modified by cardanol bisphenol A epoxide resin.Detected result: oxirane value 0.40, viscosity 32000mPa*s (25 DEG C).
With MD650 solidifying agent with the use of rear
Embodiment 2:
Cardanol 300 grams mixes through heating with dihydroxyphenyl propane 273.6 grams, under 7 grams of concentrated sulfuric acid catalyst effects, 100 DEG C are reacted 2 hours, synthesize intermediate, add epoxy chlorine again and maintain the temperature at 60 ~ 70 DEG C than 277.5 grams, alkane, drip the sodium hydroxide solution 80 grams of 30 ~ 50% mass fractions, be incubated to 80 degree of reactions 3 hours, through washing, extraction, removes water and excessive response raw material obtains target product modified by cardanol bisphenol A epoxide resin.Detected result: oxirane value 0.42, viscosity 35000mPa*s (25 DEG C).
With MD650 solidifying agent with the use of rear
Claims (3)
1. prepare the method for modified epoxy for one kind, it is characterized in that: first take cardanol and dihydroxyphenyl propane, described cardanol and the mol ratio of bis-phenol are 1:1 ~ 10, then above-mentioned cardanol and dihydroxyphenyl propane are joined in a reaction vessel, the vitriol oil is added again in described reaction vessel, the quality of the described vitriol oil is 1 ~ 7% of cardanol quality, described cardanol and dihydroxyphenyl propane synthesize intermediate under the catalysis of the vitriol oil, in intermediate, add epoxy chlorine compare alkane, described intermediate and epoxy chlorine are 1:1 ~ 10 than the mol ratio of alkane, temperature of reaction is 60 ~ 70 DEG C, drip sodium hydroxide solution again, described intermediate and sodium hydroxide mol ratio are 1:1 ~ 10, dropwise rear insulation 70 ~ 85 DEG C, react 2 ~ 4 hours, through washing, extraction, the epoxy resin of modified by cardanol dihydroxyphenyl propane is obtained after removing water and excess raw material.
2. a kind of method preparing modified epoxy according to claim 1, is characterized in that: the mass percent concentration of the described vitriol oil is 80 ~ 95%.
3. a kind of method preparing modified epoxy according to claim 1, is characterized in that: the mass fraction of described sodium hydroxide is 30 ~ 50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510142293.1A CN104725598A (en) | 2014-12-23 | 2015-03-30 | Method for preparing modified epoxy resin |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410828473 | 2014-12-23 | ||
| CN2014108284730 | 2014-12-23 | ||
| CN201510142293.1A CN104725598A (en) | 2014-12-23 | 2015-03-30 | Method for preparing modified epoxy resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104725598A true CN104725598A (en) | 2015-06-24 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510142293.1A Pending CN104725598A (en) | 2014-12-23 | 2015-03-30 | Method for preparing modified epoxy resin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237734A (en) * | 2015-11-08 | 2016-01-13 | 福建师范大学 | Synthesis method of cardanol-based epoxy resin |
| CN113683752A (en) * | 2021-10-14 | 2021-11-23 | 山东天茂新材料科技股份有限公司 | Preparation method of high-toughness epoxy resin |
| CN114773560A (en) * | 2022-04-22 | 2022-07-22 | 深圳飞扬骏研新材料股份有限公司 | Preparation method of salt-fog-resistant modified polyaspartic acid ester, salt-fog-resistant modified polyaspartic acid ester and coating |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554435A (en) * | 2013-11-20 | 2014-02-05 | 哈尔滨师范大学 | Bisphenol-A cashew phenol epoxy resin and preparation method thereof |
-
2015
- 2015-03-30 CN CN201510142293.1A patent/CN104725598A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554435A (en) * | 2013-11-20 | 2014-02-05 | 哈尔滨师范大学 | Bisphenol-A cashew phenol epoxy resin and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 贺江等: "腰果酚改性环氧树脂的研制", 《涂料工业》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237734A (en) * | 2015-11-08 | 2016-01-13 | 福建师范大学 | Synthesis method of cardanol-based epoxy resin |
| CN105237734B (en) * | 2015-11-08 | 2017-06-09 | 福建师范大学 | A kind of synthetic method of anacardol base epoxy |
| CN113683752A (en) * | 2021-10-14 | 2021-11-23 | 山东天茂新材料科技股份有限公司 | Preparation method of high-toughness epoxy resin |
| CN114773560A (en) * | 2022-04-22 | 2022-07-22 | 深圳飞扬骏研新材料股份有限公司 | Preparation method of salt-fog-resistant modified polyaspartic acid ester, salt-fog-resistant modified polyaspartic acid ester and coating |
| CN114773560B (en) * | 2022-04-22 | 2023-11-21 | 深圳飞扬骏研新材料股份有限公司 | Preparation method of salt spray resistant modified polyaspartic acid ester, salt spray resistant modified polyaspartic acid ester and coating |
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Application publication date: 20150624 |