CN109021213A - A kind of aqueous epoxy resins and preparation method thereof - Google Patents
A kind of aqueous epoxy resins and preparation method thereof Download PDFInfo
- Publication number
- CN109021213A CN109021213A CN201810599854.4A CN201810599854A CN109021213A CN 109021213 A CN109021213 A CN 109021213A CN 201810599854 A CN201810599854 A CN 201810599854A CN 109021213 A CN109021213 A CN 109021213A
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- China
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- preparation
- epoxy resin
- epoxy resins
- polyetheramine
- aqueous epoxy
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5006—Amines aliphatic
- C08G59/502—Polyalkylene polyamines
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
Abstract
The invention discloses a kind of aqueous epoxy resins and preparation method thereof.Aqueous epoxy resins of the invention the preparation method is as follows: first polyetheramine is reacted with mono-epoxy compounds, be prepared into intermediate, then intermediate and epoxy resin are condensed, obtain aqueous epoxy resins.Non-volatile point of aqueous epoxy resins of the invention, solvent-free addition, modest viscosity, preparation method is simple, has a wide range of application, and lotion storage stability prepared therefrom is good, emulsion particle diameter is small, and its paint film good toughness for being made by mixing with curing agent.
Description
Technical field
The present invention relates to a kind of aqueous epoxy resins and preparation method thereof.
Background technique
Epoxy resin is widely used because it is with excellent physical and chemical performance in coating, adhesive, composite material
Equal numerous areas.Traditional epoxy coating is mostly not soluble in water, and viscosity is larger, and it is a large amount of organic to apply man-hour requirement addition
Solvent is diluted, and can be caused damages to the health of ecological environment and construction personnel.Nearly ten years, aqueous epoxy resins
Application field it is more and more wider, in certain fields instead of oiliness epoxy resin, with people to environmental protection increasingly
Pay attention to, waterborne epoxy coatings is likely to eventually replace solvent epoxy coatings completely.Due to the performance pair of aqueous epoxy resins
The overall performance of waterborne epoxy coatings has conclusive effect, so exploitation is had excellent performance, environmentally protective water-base epoxy tree
Rouge is crucial.
Currently, water-borne modification of epoxy resin method has very much, it is roughly divided into additional emulsifier method, chemic modified method and curing agent
Emulsion process, but there is apparent defect.Additional emulsifier method needs introduce emulsifier in whole system, in final solidfied material
Remain emulsifier, will affect the physical mechanical property of solidfied material；Chemic modified method is complicated for operation, higher cost；Curing agent cream
Although change method technique is simpler than additional emulsifier method, incomplete, big, poor storage stability of dispersion particle diameter etc. that there are resin emulsifications
Problem.A certain amount of cosolvent is added in existing aqueous epoxy resins often to reduce viscosity and improve emulsion-stabilizing
Property, but also will increase the VOC content of water-based system simultaneously, and there are film poor toughness, storage for many ionic water-base resins
Stablize the problems such as bad, is difficult to meet growing actual demand.
Therefore, it is necessary to which it is tough to develop good a kind of modest viscosity, storage stability, safety and environmental protection, good emulsion stability, paint film
The good aqueous epoxy resins of property.
Summary of the invention
The purpose of the present invention is to provide a kind of aqueous epoxy resins and preparation method thereof.
The technical solution used in the present invention is:
A kind of preparation method of aqueous epoxy resins, comprising the following steps: first polyetheramine is reacted with mono-epoxy compounds,
It is prepared into intermediate, then intermediate and epoxy resin are condensed, obtains aqueous epoxy resins.
The polyetheramine is polyetheramine D230.
The mono-epoxy compounds is at least one of allyl glycidyl ether, glycidyl methacrylate.
The epoxy resin is bisphenol A type epoxy resin.
The polyetheramine, mono-epoxy compounds molar ratio be (1~1.2): 1.
The intermediate, epoxy resin mass ratio be 1:(3~10).
The beneficial effects of the present invention are: non-volatile point of aqueous epoxy resins of the invention, solvent-free addition, modest viscosity,
Preparation method is simple, has a wide range of application, and lotion storage stability prepared therefrom is good, emulsion particle diameter is small, and it is mixed with curing agent
Close the paint film good toughness being fabricated to.
1) it is related to fully meet country for non-volatile point of aqueous epoxy resins of the invention, and solvent-free addition, modest viscosity
The requirement of environmental protection；
2) aqueous epoxy resins of the invention mix the lotion being made into water, and centrifugal stability is good, and room temperature can be stablized
Storage 6 months or more；
3) the self-emulsifying excellent effect of aqueous epoxy resins of the invention, emulsion particle diameter distribution are concentrated, and emulsion particle diameter <
500 μm, lotion has blue light；
4) contain long polyether segment on aqueous epoxy resins molecule of the invention, improve the flexibility of molecule, with
The paint film impact resistance that curing agent is mixed is good, flexibility is good；
5) aqueous epoxy resins of the invention can be used for bonding, repairing and water under terrace, water conservancy projects, wet environment
The fields such as lower anticorrosive paint.
Specific embodiment
A kind of preparation method of aqueous epoxy resins, comprising the following steps: first polyetheramine is reacted with mono-epoxy compounds,
It is prepared into intermediate, then intermediate and epoxy resin are condensed, obtains aqueous epoxy resins.
Preferably, a kind of preparation method of aqueous epoxy resins, comprising the following steps: first close polyetheramine and mono-epoxide
Object mixing, 45~55 DEG C of 2~3h of reaction obtain intermediate, then intermediate is added drop-wise in epoxy resin, 80 after dripping~
110 DEG C of 2~4h of reaction, obtain aqueous epoxy resins.
Preferably, the polyetheramine is polyetheramine D230, and structural formula isx≈
2.5。
Preferably, the mono-epoxy compounds be allyl glycidyl ether, in glycidyl methacrylate extremely
Few one kind.
Preferably, the epoxy resin is bisphenol A type epoxy resin.
It is further preferred that the epoxy resin is by epoxy resin E-51, epoxy resin E-20 according to mass ratio 1:(0.2
~0.5) it compounds.
Still further preferably, the epoxy resin is by epoxy resin E-51, epoxy resin E-20 according to mass ratio 1:
(0.4~0.5) compounds.
Preferably, the polyetheramine, mono-epoxy compounds molar ratio be (1~1.2): 1.
Preferably, the intermediate, epoxy resin mass ratio be 1:(3~10).
The present invention will be further explained combined with specific embodiments below and explanation.
Embodiment 1:
First 23g polyetheramine D230 and 11.4g allyl glycidyl ether is mixed, is warming up to 50 DEG C, isothermal reaction 2h is obtained
It is mixed to intermediate, then by 59.5g epoxy resin E-51 and 25.5g epoxy resin E-20, is warming up to 80 DEG C, it is complete to epoxy resin
15g intermediate is added dropwise after full thawing, intermediate drips rear isothermal reaction 2h, obtains aqueous epoxy resins.
Embodiment 2:
First 23g polyetheramine D230 and 11.8g glycidyl methacrylate is mixed, is warming up to 50 DEG C, isothermal reaction
2.5h obtains intermediate, then 60g epoxy resin E-51 and 27g epoxy resin E-20 is mixed, and 90 DEG C is warming up to, to asphalt mixtures modified by epoxy resin
10g intermediate is added dropwise after melting completely in rouge, and intermediate drips rear isothermal reaction 3h, obtains aqueous epoxy resins.
Embodiment 3:
First 22g polyetheramine D230 and 10g allyl glycidyl ether is mixed, is warming up to 50 DEG C, isothermal reaction 3h is obtained
Intermediate, then 50g epoxy resin E-51 and 24g epoxy resin E-20 is mixed, 100 DEG C are warming up to, is melted completely to epoxy resin
20g intermediate is added dropwise after change, intermediate drips rear isothermal reaction 3.5h, obtains aqueous epoxy resins.
Embodiment 4:
First 27.5g polyetheramine D230 and 16.2g glycidyl methacrylate is mixed, is warming up to 50 DEG C, constant temperature is anti-
3h is answered, intermediate is obtained, then 54g epoxy resin E-51 and 27g epoxy resin E-20 is mixed, 110 DEG C is warming up to, to asphalt mixtures modified by epoxy resin
10g intermediate is added dropwise after melting completely in rouge, and intermediate drips rear isothermal reaction 4h, obtains aqueous epoxy resins.
Embodiment 5:
First 27.5g polyetheramine D230 and 11.4g allyl glycidyl ether is mixed, is warming up to 50 DEG C, isothermal reaction
2.5h obtains intermediate, then 54g epoxy resin E-51 and 27g epoxy resin E-20 is mixed, and 95 DEG C is warming up to, to asphalt mixtures modified by epoxy resin
10g intermediate is added dropwise after melting completely in rouge, and intermediate drips rear isothermal reaction 4h, obtains aqueous epoxy resins.
Test case:
1) aqueous epoxy resins prepared by Examples 1 to 5 are warming up to 50 DEG C, are slowly added distilled water, whole system
The trend of first increases and then decreases can be presented in viscosity, and the adding speed of distilled water is improved when viscosity starts to become smaller, until solid content
Reach 60%, obtain water-based emulsion 1~5, then be tested for the property to water-based emulsion, test result is as follows shown in table:
The performance test results of 1 water-based emulsion 1~5 of table
Note:
The test method of each performance indicator is as follows in table:
Centrifugal stability: water-based emulsion is added in centrifuge, and adjustment revolving speed to 3000r/min is centrifuged 30min, then sees
Survey whether lotion phenomena such as layering, flocculation sedimentation occurs；
Storage stability: by water-based emulsion room temperature 6 months, then observe whether lotion phenomena such as sedimentation, layering occurs.
2) water-based emulsion 1~5 and waterborne curing agent are mixed and made into varnish, and are fabricated to epoxy resin varnish paint film (paint
Film sample 1~5), then varnish paint film room temperature is stood into 30min, place into 70 DEG C of curing oven 1h, natural cooling, then progressive
It can test, test result is as follows shown in table:
The performance test results of 2 paint film sample 1~5 of table
Note:
The test method of each performance indicator is as follows in table:
Pencil hardness: it by the pencil of certain degree of hardness label on pencil hardometer, is streaked on film, examines lead
Whether pen core generates scratch on film, indicates film pencil hardness with the most hard pencil label that does not cause film to destroy,
According to the regulation of GB/T 6739-1996, pencil hardness is by totally 13 grades of 6H to 6B, and wherein 6H is most hard, and 6B is most soft, and hardness of film is
It is indicated with corresponding pencil hardness；
Adhesive force (cross-hatching): marking square cross checker pattern at equal intervals with Checker marking knife on coating, between grid
Away from for 1mm, scratch should penetrate film until ground, sticks 3M adhesive tape drawing a lattice region, make it with the pressing adhesive tape of finger gently
It is come into full contact with the film for drawing lattice region, then pulls open adhesive tape rapidly, observation draws whether lattice region has coating to be glued from substrate.It presses
Measurement result can be classified according to GB/T 9286-1998 " cross cut test of paint and varnish paint film ", the adhesive force of film
Grade be divided into six ranks from 0 grade to 5, none completely smooth lattice of 0 grade of expression cut edge fall off, 5 grades indicate 65% or more area
Domain coating falls off；
Flexibility (shaft rod bending test): the coating test plate (panel) made being placed on the circular shaft of known diameter and is bent, observation
The cracking of coating destroys situation.According to the regulation of GB/T6742-86 " paint film bend test (cylindrical shaft) ", film it is flexible
Property indicated with the minimum mandrel rod diameter for not causing film to destroy；
Impact resistance height: it is measured according to GB/T 1732-93 " paint film impact resistance measuring method ".The iron plate of film is set
In on anvil, film is placed upward, and certain altitude places the weight of fixed mass right above film, pounds weight free-falling
On film and iron plate, then with amplification sem observation paint film either with or without cracked and peeling phenomenon, paint film impact resistance is not with drawing
The maximum height that the weight that paint film destroys is placed indicates.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of aqueous epoxy resins, it is characterised in that: the following steps are included: first by polyetheramine and mono-epoxide
Object reaction is closed, intermediate is prepared into, then intermediate and epoxy resin are condensed, obtains aqueous epoxy resins.
2. preparation method according to claim 1, it is characterised in that: the following steps are included: first by polyetheramine and monocycle oxygen
Compound mixing, 45~55 DEG C of 2~3h of reaction obtain intermediate, then intermediate is added drop-wise in epoxy resin, 80 after dripping
~110 DEG C of 2~4h of reaction, obtain aqueous epoxy resins.
3. preparation method according to claim 1 or 2, it is characterised in that: the polyetheramine is polyetheramine D230.
4. preparation method according to claim 1 or 2, it is characterised in that: the mono-epoxy compounds is allyl glycidyl
At least one of glycerin ether, glycidyl methacrylate.
5. preparation method according to claim 1 or 2, it is characterised in that: the epoxy resin is bisphenol type epoxy tree
Rouge.
6. preparation method according to claim 5, it is characterised in that: the epoxy resin is by epoxy resin E-51, epoxy
Resin E-20 is according to mass ratio 1:(0.2~0.5) it compounds.
7. preparation method according to claim 1 or 2, it is characterised in that: mole of the polyetheramine, mono-epoxy compounds
Than for (1~1.2): 1.
8. preparation method according to claim 1 or 2, it is characterised in that: the intermediate, epoxy resin mass ratio be
1:(3~10).
9. the aqueous epoxy resins that preparation method of any of claims 1 or 2 is prepared.
10. aqueous epoxy resins as claimed in claim 9 are in the application in aqueous floor paint, water-based anticorrosive paint field.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810599854.4A CN109021213B (en) | 2018-06-12 | 2018-06-12 | Water-based epoxy resin and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810599854.4A CN109021213B (en) | 2018-06-12 | 2018-06-12 | Water-based epoxy resin and preparation method thereof |
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| CN109021213A true CN109021213A (en) | 2018-12-18 |
| CN109021213B CN109021213B (en) | 2020-12-15 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111836864A (en) * | 2020-05-28 | 2020-10-27 | 江苏扬农锦湖化工有限公司 | Water-based epoxy floor paint and preparation method thereof |
| CN112680105A (en) * | 2020-12-28 | 2021-04-20 | 大连油漆有限公司 | Environment-friendly anticorrosive paint, hyperbranched epoxy resin and preparation method thereof |
| CN114686069A (en) * | 2020-12-28 | 2022-07-01 | 中海油常州涂料化工研究院有限公司 | Polyacrylate resin modified waterborne epoxy emulsion and preparation method thereof |
| WO2023121073A1 (en) * | 2021-12-20 | 2023-06-29 | 한국화학연구원 | Gemini-type epoxy resin emulsifier and method for preparing same |
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| CN106987194A (en) * | 2017-04-14 | 2017-07-28 | 华南理工大学 | A kind of non-ion aqueous epoxy resin latex and nonionic waterborne epoxy curing agent and its preparation method and aqueous epoxy resins varnish |
| CN108003755A (en) * | 2017-12-25 | 2018-05-08 | 昆明国松特种涂料有限公司 | A kind of non-solvent epoxy drinking-water white paint and preparation method thereof |
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Patent Citations (4)
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| WO2011024014A1 (en) * | 2009-08-27 | 2011-03-03 | Polinvent Kft. | Amine-epoxy adducts and their use for preparing polyurea and polyurea-polyurethane coatings |
| CN102633989A (en) * | 2012-03-27 | 2012-08-15 | 广东新劲刚超硬材料有限公司 | Non-ionic active epoxy emulsifier preparation method and waterborne epoxy resin preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111836864A (en) * | 2020-05-28 | 2020-10-27 | 江苏扬农锦湖化工有限公司 | Water-based epoxy floor paint and preparation method thereof |
| WO2021237556A1 (en) * | 2020-05-28 | 2021-12-02 | 江苏扬农锦湖化工有限公司 | Waterborne epoxy floor paint and preparation method therefor |
| CN112680105A (en) * | 2020-12-28 | 2021-04-20 | 大连油漆有限公司 | Environment-friendly anticorrosive paint, hyperbranched epoxy resin and preparation method thereof |
| CN114686069A (en) * | 2020-12-28 | 2022-07-01 | 中海油常州涂料化工研究院有限公司 | Polyacrylate resin modified waterborne epoxy emulsion and preparation method thereof |
| WO2023121073A1 (en) * | 2021-12-20 | 2023-06-29 | 한국화학연구원 | Gemini-type epoxy resin emulsifier and method for preparing same |
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| CN109021213B (en) | 2020-12-15 |
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