CN110396177A - A kind of low viscosity aqueous epoxy resin and the preparation method and application thereof - Google Patents
A kind of low viscosity aqueous epoxy resin and the preparation method and application thereof Download PDFInfo
- Publication number
- CN110396177A CN110396177A CN201910343947.5A CN201910343947A CN110396177A CN 110396177 A CN110396177 A CN 110396177A CN 201910343947 A CN201910343947 A CN 201910343947A CN 110396177 A CN110396177 A CN 110396177A
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- low viscosity
- epoxy resin
- aqueous epoxy
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- viscosity aqueous
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/12—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms
- C07D303/18—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms by etherified hydroxyl radicals
- C07D303/20—Ethers with hydroxy compounds containing no oxirane rings
- C07D303/24—Ethers with hydroxy compounds containing no oxirane rings with polyhydroxy compounds
- C07D303/27—Ethers with hydroxy compounds containing no oxirane rings with polyhydroxy compounds having all hydroxyl radicals etherified with oxirane containing compounds
-
- 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
- C08G59/20—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 epoxy compounds used
- C08G59/22—Di-epoxy compounds
- C08G59/24—Di-epoxy compounds carbocyclic
- C08G59/245—Di-epoxy compounds carbocyclic aromatic
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Epoxy Resins (AREA)
- Epoxy Compounds (AREA)
Abstract
A kind of low viscosity aqueous epoxy resin provided by the invention, the present invention also provides a kind of preparation methods of low viscosity aqueous epoxy resin, in the presence of sodium hydroxide, Formulas I compound represented and excessive epoxychloropropane polymerization reaction to get.Waterborne epoxy coatings provided by the invention is by studying different aqueous epoxy resins, zero VOC, large arch dam waterborne epoxy coatings is prepared, realize the technology of water paint high solid low viscosity, break through high solid solvent based coating can not Water-borne modification technical problem, it is further reduced VOC emission, meet national environmental protection policy, the industry that can need to provide heavy antisepsis for harbour machinery, ship and ocean platform etc. provides good protection.
Description
Technical field
The present invention relates to coating material field, in particular to a kind of low viscosity aqueous epoxy resin and preparation method thereof with answer
With.
Background technique
Due to water-base resin material viscosity is high and high speed dispersion is easy to cause resin demulsification etc., water-base epoxy at present
The technique that water defibrination is widely used in coating in the fabrication process.The technique is cumbersome, and the manufacturing cycle is long, and energy consumption is high, manufacturing process
Middle needs add the auxiliary agent containing VOC, need additional water, cause the solid content of product low, and when coating application needs repeatedly to apply
Dress can be only achieved ideal effect, and energy consumption is high, and the period is long, and the water paint produced by the technique can only substitute oil product
VOC is greater than the coating of 420g/L, cannot substitute other oil products for containing VOC (VOC is less than 420g/L).Further to drop
Energy consumption and discharge of poisonous waste in low production process promote waterborne epoxy coatings quality, realize green production, need to painting
Material manufacturing technique improves.
Summary of the invention
Technical problem: in order to solve the defects of prior art, the present invention provides a kind of low viscosity aqueous epoxy resin and
Preparation method and application.
Technical solution: a kind of low viscosity aqueous epoxy resin provided by the invention, structural formula are as follows:
Wherein, R1-R11It is independently H, halogen, alkyl, naphthenic base, aryl, hydroxyl, ether, aliphatic radical.
The present invention also provides a kind of low viscosity aqueous epoxy resin, structural formula is as follows:
The present invention also provides a kind of preparation methods of low viscosity aqueous epoxy resin, comprising the following steps: in hydroxide
In the presence of sodium, Formulas I compound represented and excessive epoxychloropropane polymerization reaction to get；Reaction equation is as follows:
Formulas I compound represented and epoxychloropropane stir and heat, hydroxide is added dropwise when temperature is raised to 60-70 DEG C
Sodium water solution is added dropwise at 70-80 DEG C in 2 hours；It improves temperature and obtains sticky tree in 90-100 DEG C of holding 1-2h
Rouge；Distilled water and toluene are added in viscous resin, stirring dissolves resin, and static layering removes water layer, and toluene layer decompression is steamed
It is dry to get.
Formulas I compound represented and the molar ratio of epoxychloropropane are n:(2n+2 to 2n+4).
The content of sodium hydroxide is 0.5n-1.5n moles in sodium hydrate aqueous solution.
The volume ratio of distilled water and toluene is 1:2.
The present invention also provides a kind of preparation methods of low viscosity aqueous epoxy resin, in the presence of sodium hydroxide, Formula II
Compound represented and excessive epoxychloropropane polymerization reaction to get；Reaction equation is as follows:
Formulas I compound represented and epoxychloropropane stir and heat, hydroxide is added dropwise when temperature is raised to 60-70 DEG C
Sodium water solution is added dropwise at 70-80 DEG C in 2 hours；It improves temperature and obtains sticky tree in 90-100 DEG C of holding 1-2h
Rouge；Distilled water and toluene are added in viscous resin, stirring dissolves resin, and static layering removes water layer, and toluene layer decompression is steamed
It is dry to get；Formulas I compound represented and the molar ratio of epoxychloropropane are n:(2n+2 to 2n+4)；In sodium hydrate aqueous solution
The content of sodium hydroxide is 0.5n-1.5n moles；The volume ratio of distilled water and toluene is 1:2.
Application of the above-mentioned low viscosity aqueous epoxy resin in aqueous epoxide resin paint.
The utility model has the advantages that waterborne epoxy coatings provided by the invention is prepared by studying different aqueous epoxy resins
Zero VOC, large arch dam waterborne epoxy coatings realize the technology of water paint high solid low viscosity, break through high solid solvent type and apply
Material can not Water-borne modification technical problem, be further reduced VOC emission, meet national environmental protection policy, can be harbour machinery, ship
The industry that oceangoing ship and ocean platform etc. need to provide heavy antisepsis provides good protection.
Detailed description of the invention
Fig. 1 is the hydrogen spectrogram of aqueous epoxy resins produced by the present invention.
Specific embodiment
The present invention is further illustrated below.
Embodiment 1
Formula II compound represented and epoxychloropropane stir and heat, hydrogen-oxygen is added dropwise when temperature is raised to 60-70 DEG C
Change sodium water solution, is added dropwise at 70-80 DEG C in 2 hours；It improves temperature and obtains sticky tree in 90-100 DEG C of holding 1-2h
Rouge；Distilled water and toluene are added in viscous resin, stirring dissolves resin, and static layering removes water layer, and toluene layer decompression is steamed
It is dry to get；Formulas I compound represented and the molar ratio of epoxychloropropane are n:(2n+2 to 2n+4)；In sodium hydrate aqueous solution
The content of sodium hydroxide is 0.5n-1.5n moles；The volume ratio of distilled water and toluene is 1:2.
Reaction product 408g, m/z=422.2 are obtained, hydrogen spectrum is shown in Fig. 1.
Embodiment 2
Formula II compound represented and epoxychloropropane stir and heat, hydrogen-oxygen is added dropwise when temperature is raised to 60-70 DEG C
Change sodium water solution, is added dropwise at 70-80 DEG C in 2 hours；It improves temperature and obtains sticky tree in 90-100 DEG C of holding 1-2h
Rouge；Distilled water and toluene are added in viscous resin, stirring dissolves resin, and static layering removes water layer, and toluene layer decompression is steamed
It is dry to get；Formulas I compound represented and the molar ratio of epoxychloropropane are n:(2n+2 to 2n+4)；In sodium hydrate aqueous solution
The content of sodium hydroxide is 0.5n-1.5n moles；The volume ratio of distilled water and toluene is 1:2.
Reaction product 395g, m/z=422.2 are obtained, hydrogen spectrum is shown in Fig. 1.
Embodiment 3
Formula II compound represented and epoxychloropropane stir and heat, hydrogen-oxygen is added dropwise when temperature is raised to 60-70 DEG C
Change sodium water solution, is added dropwise at 70-80 DEG C in 2 hours；It improves temperature and obtains sticky tree in 90-100 DEG C of holding 1-2h
Rouge；Distilled water and toluene are added in viscous resin, stirring dissolves resin, and static layering removes water layer, and toluene layer decompression is steamed
It is dry to get；Formulas I compound represented and the molar ratio of epoxychloropropane are n:(2n+2 to 2n+4)；In sodium hydrate aqueous solution
The content of sodium hydroxide is 0.5n-1.5n moles；The volume ratio of distilled water and toluene is 1:2.
Reaction product 392g, m/z=422.2 are obtained, hydrogen spectrum is shown in Fig. 1.
The preparation of 4 waterborne epoxy coatings of embodiment
A batch waterborne epoxy coatings, formula such as following table is made.
The performance for testing above-mentioned waterborne epoxy coatings, as a result see the table below.
| Number | Viscosity (applies -4 glasss, s) | Solid part % | Coating thickness | VOC |
| Sample 1 | 23±2 | 80 | 106 | 167 |
| Sample 2 | 22±2 | 81 | 107 | 165 |
Claims (10)
1. a kind of low viscosity aqueous epoxy resin, structural formula are as follows:
Wherein, R1-R11It is independently H, halogen, alkyl, naphthenic base, aryl, hydroxyl, ether, aliphatic radical.
2. a kind of low viscosity aqueous epoxy resin, structural formula are as follows:
3. a kind of preparation method of low viscosity aqueous epoxy resin, it is characterised in that: the following steps are included: existing in sodium hydroxide
Under, Formulas I compound represented and excessive epoxychloropropane polymerization reaction to get；Reaction equation is as follows:
4. a kind of preparation method of low viscosity aqueous epoxy resin according to claim 3, it is characterised in that: shown in Formulas I
Compound and epoxychloropropane, stir and heat, sodium hydrate aqueous solution is added dropwise when temperature is raised to 60-70 DEG C, in 70-80
It is added dropwise at DEG C in 2 hours；It improves temperature and obtains viscous resin in 90-100 DEG C of holding 1-2h；It is added and steams in viscous resin
Distilled water and toluene, stirring dissolve resin, static layering remove water layer, toluene layer evaporated under reduced pressure to get.
5. a kind of preparation method of low viscosity aqueous epoxy resin according to claim 2, it is characterised in that: shown in Formulas I
Compound and epoxychloropropane molar ratio be n:(2n+2 to 2n+4).
6. a kind of preparation method of low viscosity aqueous epoxy resin according to claim 2, it is characterised in that: sodium hydroxide
The content of sodium hydroxide is 0.5n-1.5n moles in aqueous solution.
7. a kind of preparation method of low viscosity aqueous epoxy resin according to claim 2, it is characterised in that: distilled water and
The volume ratio of toluene is 1:2.
8. a kind of preparation method of low viscosity aqueous epoxy resin according to claim 2, it is characterised in that: in hydroxide
In the presence of sodium, Formula II compound represented and excessive epoxychloropropane polymerization reaction to get；Reaction equation is as follows:
9. a kind of preparation method of low viscosity aqueous epoxy resin according to claim 2, it is characterised in that: shown in Formulas I
Compound and epoxychloropropane, stir and heat, sodium hydrate aqueous solution is added dropwise when temperature is raised to 60-70 DEG C, in 70-80
It is added dropwise at DEG C in 2 hours；It improves temperature and obtains viscous resin in 90-100 DEG C of holding 1-2h；It is added and steams in viscous resin
Distilled water and toluene, stirring dissolve resin, static layering remove water layer, toluene layer evaporated under reduced pressure to get；Chemical combination shown in Formulas I
The molar ratio of object and epoxychloropropane is n:(2n+2 to 2n+4)；The content of sodium hydroxide is 0.5n- in sodium hydrate aqueous solution
1.5n mole；The volume ratio of distilled water and toluene is 1:2.
10. application of the low viscosity aqueous epoxy resin described in claim 1 in aqueous epoxide resin paint.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910343947.5A CN110396177A (en) | 2019-04-26 | 2019-04-26 | A kind of low viscosity aqueous epoxy resin and the preparation method and application thereof |
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| CN201910343947.5A CN110396177A (en) | 2019-04-26 | 2019-04-26 | A kind of low viscosity aqueous epoxy resin and the preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112759741A (en) * | 2020-12-18 | 2021-05-07 | 上海瀚岱化学有限公司 | High-stability water-based epoxy resin and preparation method thereof |
| CN113214452A (en) * | 2020-01-21 | 2021-08-06 | 山东圣泉新材料股份有限公司 | Epoxy resin and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101117376A (en) * | 2007-09-12 | 2008-02-06 | 大连齐化化工有限公司 | Low-viscosity bisphenol A epoxide resin and production method thereof |
| CN103613739A (en) * | 2013-11-18 | 2014-03-05 | 山东圣泉化工股份有限公司 | Method for preparing epoxy resin |
| CN106536589A (en) * | 2014-07-22 | 2017-03-22 | 沙特基础工业全球技术有限公司 | High heat monomers and methods of use thereof |
| CN107828311A (en) * | 2017-11-27 | 2018-03-23 | 陕西启源科技发展有限责任公司 | The preparation method of aqueous epoxide resin paint |
-
2019
- 2019-04-26 CN CN201910343947.5A patent/CN110396177A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101117376A (en) * | 2007-09-12 | 2008-02-06 | 大连齐化化工有限公司 | Low-viscosity bisphenol A epoxide resin and production method thereof |
| CN103613739A (en) * | 2013-11-18 | 2014-03-05 | 山东圣泉化工股份有限公司 | Method for preparing epoxy resin |
| CN106536589A (en) * | 2014-07-22 | 2017-03-22 | 沙特基础工业全球技术有限公司 | High heat monomers and methods of use thereof |
| CN107828311A (en) * | 2017-11-27 | 2018-03-23 | 陕西启源科技发展有限责任公司 | The preparation method of aqueous epoxide resin paint |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113214452A (en) * | 2020-01-21 | 2021-08-06 | 山东圣泉新材料股份有限公司 | Epoxy resin and preparation method and application thereof |
| CN112759741A (en) * | 2020-12-18 | 2021-05-07 | 上海瀚岱化学有限公司 | High-stability water-based epoxy resin and preparation method thereof |
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