CN104558520A - Synthesis method of silica sol modified epoxy resin - Google Patents
Synthesis method of silica sol modified epoxy resin Download PDFInfo
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- CN104558520A CN104558520A CN201410579623.9A CN201410579623A CN104558520A CN 104558520 A CN104558520 A CN 104558520A CN 201410579623 A CN201410579623 A CN 201410579623A CN 104558520 A CN104558520 A CN 104558520A
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- epoxy resin
- silica sol
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Abstract
The invention relates to a synthesis method of a silica sol modified epoxy resin. The synthesis method comprises the following steps: adding ethyl orthosilicate and ethanol to a 3-neck boiling flask, and meanwhile, stirring, and adding a mixed solution of hydrochloric acid and deionized water to have a hydrolysis reaction to obtain silica sol; adding a proper amount of ethyl acetate, butyl acetate, cyclohexanone, epoxy resin E-44 pre-dissolved in acetone and a catalyst to the 3-neck boiling flask in which a stirrer is loaded and from which air is exhausted, and then adding the silica sol in batches; and reacting at a constant temperature, removing the solvent, and finally obtaining the silica sol modified epoxy resin. The synthesis method is simple, low in cost, and free from addition of a curing agent; and the synthesized silica sol modified epoxy resin has excellent mechanical properties, corrosion resistance and heat resistance.
Description
Technical field
The present invention relates to a kind of synthetic technology of organic coating, particularly relate to a kind of silica sol modified epoxy resin synthetic method.
Background technology
Epoxy resin is that general reference is containing more than 2 or 2 epoxy group(ing), the high-molecular oligomers body of thermoset products is formed by epoxide group reaction for skeleton with organic compound such as aliphatics, alicyclic or aromatic series, it has excellent cohesiveness, electrical insulating property, mechanical property, erosion resistance etc., be used widely in many fields of national economy, but the thermotolerance of epoxy resin and shock-resistance poor, limit its range of application.
Summary of the invention
It is simple that technical problem to be solved by this invention is to provide a kind of method, and with low cost, without the need to adding solidifying agent, the silica sol modified epoxy resin of synthesis has good mechanical property, the synthetic method of corrosion resistance nature and resistance toheat.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of silica sol modified epoxy resin synthetic method, comprises the steps:
Tetraethoxy, ethanol are added in there-necked flask, and stir simultaneously, drip the mixing solutions of hydrochloric acid and deionized water, constant temperature is hydrolyzed reaction, obtains silicon sol;
Be equipped with in the there-necked flask of agitator, excluding air, add appropriate ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer, then add silicon sol in batches;
Isothermal reaction, pumps solvent, obtains silica sol modified epoxy resin.
On the basis of technique scheme, the present invention can also do following improvement.
Further, describedly tetraethoxy, ethanol to be added in there-necked flask, and stir simultaneously, drip the mixing solutions of hydrochloric acid and deionized water, constant temperature is hydrolyzed reaction, obtains being implemented as follows of silicon sol step:
Tetraethoxy, ethanol are added in there-necked flask, and stir 10 ~ 30min simultaneously, dripping volume ratio is the hydrochloric acid of 1:1 ~ 1:3 and the mixing solutions of deionized water, and under 80 ~ 85 DEG C of temperature condition, constant temperature is hydrolyzed reaction 1 ~ 1.5h, obtained silicon sol.
Further, described in be equipped with in the there-necked flask of agitator, excluding air, add appropriate ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer, then add being implemented as follows of silicon sol step in batches:
Be equipped with in the there-necked flask of agitator, excluding air, be that 1:1:1:1:1 ~ 1:1:1:1:1.3 adds ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer according to volume ratio, add silicon sol according to 10 ~ 12% of total mass mark in batches.
Further, described isothermal reaction, pumps solvent, obtains being implemented as follows of silica sol modified epoxy resin step:
Under 60 ~ 70 DEG C of temperature condition, isothermal reaction 1 ~ 2h, pumps solvent, utilizes 100 ~ 200 object screen filtrations, obtains silica sol modified epoxy resin.
The invention has the beneficial effects as follows: method is simple, and with low cost, without the need to adding solidifying agent, the silica sol modified epoxy resin of synthesis has good mechanical property, corrosion resistance nature and resistance toheat.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A kind of silica sol modified epoxy resin synthetic method, comprises the steps:
Tetraethoxy, ethanol are added in there-necked flask, and stir simultaneously, drip the mixing solutions of hydrochloric acid and deionized water, constant temperature is hydrolyzed reaction, obtains silicon sol;
Be equipped with in the there-necked flask of agitator, excluding air, add appropriate ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer, then add silicon sol in batches;
Isothermal reaction, pumps solvent, obtains silica sol modified epoxy resin.
Embodiment 1:
Tetraethoxy, ethanol are added in there-necked flask, and stir 10min simultaneously, dripping volume ratio is the hydrochloric acid of 1:1 and the mixing solutions of deionized water, and under 80 DEG C of temperature condition, constant temperature is hydrolyzed and reacts 1h, obtained silicon sol; Be equipped with in the there-necked flask of agitator, excluding air, be that 1:1:1:1:1 adds ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer according to volume ratio, add silicon sol according to 10% of total mass mark in batches; Under 60 DEG C of temperature condition, isothermal reaction 1h, pumps solvent, utilizes 100 object screen filtrations, obtains silica sol modified epoxy resin.
Embodiment 2:
Tetraethoxy, ethanol are added in there-necked flask, and stir 20min simultaneously, dripping volume ratio is the hydrochloric acid of 1:2 and the mixing solutions of deionized water, and under 82 DEG C of temperature condition, constant temperature is hydrolyzed and reacts 1.2h, obtained silicon sol; Be equipped with in the there-necked flask of agitator, excluding air, be that 1:1:1:1:1.2 adds ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer according to volume ratio, add silicon sol according to 11% of total mass mark in batches; Under 65 DEG C of temperature condition, isothermal reaction 1.5h, pumps solvent, utilizes 150 object screen filtrations, obtains silica sol modified epoxy resin.
Embodiment 3:
Tetraethoxy, ethanol are added in there-necked flask, and stir 30min simultaneously, dripping volume ratio is the hydrochloric acid of 1:3 and the mixing solutions of deionized water, and under 85 DEG C of temperature condition, constant temperature is hydrolyzed and reacts 1.5h, obtained silicon sol; Be equipped with in the there-necked flask of agitator, excluding air, be that 1:1:1:1:1.3 adds ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer according to volume ratio, add silicon sol according to 12% of total mass mark in batches; Under 70 DEG C of temperature condition, isothermal reaction 2h, pumps solvent, utilizes 200 object screen filtrations, obtains silica sol modified epoxy resin.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. a silica sol modified epoxy resin synthetic method, is characterized in that, comprise the steps:
Tetraethoxy, ethanol are added in there-necked flask, and stir simultaneously, drip the mixing solutions of hydrochloric acid and deionized water, constant temperature is hydrolyzed reaction, obtains silicon sol;
Be equipped with in the there-necked flask of agitator, excluding air, add appropriate ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer, then add silicon sol in batches;
Isothermal reaction, pumps solvent, obtains silica sol modified epoxy resin.
2. a kind of silica sol modified epoxy resin synthetic method according to claim 1, it is characterized in that, described tetraethoxy, ethanol are added in there-necked flask, and stir simultaneously, drip the mixing solutions of hydrochloric acid and deionized water, constant temperature is hydrolyzed reaction, being implemented as follows of obtained silicon sol step:
Tetraethoxy, ethanol are added in there-necked flask, and stir 10 ~ 30min simultaneously, dripping volume ratio is the hydrochloric acid of 1:1 ~ 1:3 and the mixing solutions of deionized water, and under 80 ~ 85 DEG C of temperature condition, constant temperature is hydrolyzed reaction 1 ~ 1.5h, obtained silicon sol.
3. a kind of silica sol modified epoxy resin synthetic method according to claim 1, it is characterized in that, describedly be equipped with in the there-necked flask of agitator, excluding air, add appropriate ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer, then add being implemented as follows of silicon sol step in batches:
Be equipped with in the there-necked flask of agitator, excluding air, be that 1:1:1:1:1 ~ 1:1:1:1:1.3 adds ethyl acetate, butylacetate, pimelinketone, acetone epoxy resin E-44 solvent in advance and catalyzer according to volume ratio, add silicon sol according to 10 ~ 12% of total mass mark in batches.
4. a kind of silica sol modified epoxy resin synthetic method according to claim 1, it is characterized in that, described isothermal reaction, pumps solvent, obtains being implemented as follows of silica sol modified epoxy resin step:
Under 60 ~ 70 DEG C of temperature condition, isothermal reaction 1 ~ 2h, pumps solvent, utilizes 100 ~ 200 object screen filtrations, obtains silica sol modified epoxy resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410579623.9A CN104558520A (en) | 2014-10-25 | 2014-10-25 | Synthesis method of silica sol modified epoxy resin |
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| CN201410579623.9A CN104558520A (en) | 2014-10-25 | 2014-10-25 | Synthesis method of silica sol modified epoxy resin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105925141A (en) * | 2016-06-23 | 2016-09-07 | 安庆市银瑞商贸有限公司 | Surface anti-corrosion heat-resistant paint for communication equipment casing |
| CN108172323A (en) * | 2016-12-22 | 2018-06-15 | 郑州电力高等专科学校 | A kind of insulated electric conductor with insulating lacquer layer |
| CN109504238A (en) * | 2018-11-23 | 2019-03-22 | 华南理工大学 | A kind of one-component self-curing chromium-free zinc aluminum anticorrosive paint and preparation and application |
| CN110079195A (en) * | 2019-05-24 | 2019-08-02 | 上海瀚岱化学有限公司 | A kind of aqueous epoxy resins composition and its application |
| CN111073510A (en) * | 2019-12-31 | 2020-04-28 | 浙江大学 | Hydrophobic and oleophobic self-cleaning material and preparation method and application thereof |
| CN113461907A (en) * | 2021-06-28 | 2021-10-01 | 中车青岛四方机车车辆股份有限公司 | Flame-retardant epoxy resin and preparation method and application thereof |
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2014
- 2014-10-25 CN CN201410579623.9A patent/CN104558520A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105925141A (en) * | 2016-06-23 | 2016-09-07 | 安庆市银瑞商贸有限公司 | Surface anti-corrosion heat-resistant paint for communication equipment casing |
| CN108172323A (en) * | 2016-12-22 | 2018-06-15 | 郑州电力高等专科学校 | A kind of insulated electric conductor with insulating lacquer layer |
| CN108172323B (en) * | 2016-12-22 | 2019-05-07 | 郑州电力高等专科学校 | A kind of insulated electric conductor with insulating lacquer layer |
| CN109504238A (en) * | 2018-11-23 | 2019-03-22 | 华南理工大学 | A kind of one-component self-curing chromium-free zinc aluminum anticorrosive paint and preparation and application |
| CN109504238B (en) * | 2018-11-23 | 2021-06-08 | 华南理工大学 | Single-component self-curing chromium-free zinc-aluminum anticorrosive paint and preparation and application thereof |
| CN110079195A (en) * | 2019-05-24 | 2019-08-02 | 上海瀚岱化学有限公司 | A kind of aqueous epoxy resins composition and its application |
| CN111073510A (en) * | 2019-12-31 | 2020-04-28 | 浙江大学 | Hydrophobic and oleophobic self-cleaning material and preparation method and application thereof |
| CN111073510B (en) * | 2019-12-31 | 2021-02-19 | 浙江大学 | Hydrophobic and oleophobic self-cleaning material and preparation method and application thereof |
| CN113461907A (en) * | 2021-06-28 | 2021-10-01 | 中车青岛四方机车车辆股份有限公司 | Flame-retardant epoxy resin and preparation method and application thereof |
| CN113461907B (en) * | 2021-06-28 | 2023-11-21 | 中车青岛四方机车车辆股份有限公司 | Flame-retardant epoxy resin and preparation method and application thereof |
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Application publication date: 20150429 |