CN110776605B - Low-VOC (volatile organic compound) water-based epoxy emulsion and preparation method thereof - Google Patents
Low-VOC (volatile organic compound) water-based epoxy emulsion and preparation method thereof Download PDFInfo
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- CN110776605B CN110776605B CN201911179641.7A CN201911179641A CN110776605B CN 110776605 B CN110776605 B CN 110776605B CN 201911179641 A CN201911179641 A CN 201911179641A CN 110776605 B CN110776605 B CN 110776605B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
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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
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention belongs to the field of high polymer materials. The low-VOC aqueous epoxy emulsion is prepared from the following components: epoxy resin, methyl vinyl dimethoxysilane, an initiator, a reactive emulsifier, an acrylate monomer, an epoxy diluent and water; the reactive emulsifier is prepared from the following components: epoxy resin, maleic acid mono polyethylene glycol monomethyl ether ester and an alkaline catalyst. The water-based epoxy emulsion disclosed by the invention is low in viscosity, small in particle size, good in dispersity, stability, water resistance and flexibility, free of organic volatile matters, environment-friendly and pollution-free.
Description
Technical Field
The invention belongs to the field of high polymer materials, and relates to a low-VOC aqueous epoxy emulsion and a preparation method thereof.
Background
The traditional epoxy resin has good adhesive force, wear resistance, scratch resistance and chemical resistance, low curing shrinkage and excellent solvent property, and is widely applied to the fields of adhesives, coatings, terraces and the like. However, in the conventional epoxy resin, a large amount of organic solvents such as alcohols, ethers and ketones are required to be diluted during construction, and a large amount of organic volatile matters not only pollute the environment, but also seriously harm the health of human bodies, so that the development of a low-VOC (volatile organic compound) water-based epoxy resin system and related coating products thereof becomes a new research direction.
Disclosure of Invention
The invention aims to solve the technical problem of providing the low-VOC aqueous epoxy emulsion which has low viscosity, small particle size, good dispersibility, stability, water resistance and flexibility, no organic volatile matter, environmental protection and no pollution.
The technical scheme of the invention is as follows:
the low-VOC aqueous epoxy emulsion is prepared from the following components in percentage by weight:
35 to 45 percent of epoxy resin,
1 to 2 percent of methyl vinyl dimethoxy silane,
0.1 to 1.2 percent of initiator,
0.5 to 2 percent of reactive emulsifier,
3 to 5 percent of acrylate monomer,
2 to 3.5 percent of epoxy diluent,
40-60% of water;
the reactive emulsifier is prepared from the following components in percentage by weight:
25 to 40 percent of epoxy resin,
58-75% of maleic acid mono-polyethylene glycol mono-methyl ether ester,
1-2% of alkaline catalyst.
Further, the epoxy resin is phenol-aralkyl type epoxy resin and triphenol methane type epoxy resin.
Further, the initiator is one of ammonium persulfate, potassium persulfate and sodium persulfate.
Further, the acrylate monomer is at least one of methyl acrylate, butyl methacrylate, ethyl acrylate or isooctyl methacrylate.
Further, the epoxy diluent is octyl glycidyl ether or trimethylolpropane triglycidyl ether.
Further, the alkaline catalyst is at least one of N, N-dimethylbenzylamine, triethanolamine salt, 2-methyl-3 imidazole, N-dimethylethanolamine, tetramethylammonium bromide, tetramethylammonium chloride, tetraethylammonium bromide, tetraethylammonium chloride, tetrabutylammonium chloride, benzyltriethylammonium chloride and hexadecyltrimethylammonium bromide.
The preparation method of the low-VOC aqueous epoxy emulsion comprises the following steps:
s1, mixing epoxy resin, maleic acid mono-polyethylene glycol monomethyl ether ester and an alkaline catalyst, and reacting at the temperature of 180 ℃ and 220 ℃ for 5-8h to obtain a reactive emulsifier;
s2, uniformly mixing an initiator, a reactive emulsifier and water, adding epoxy resin, an epoxy diluent, methyl vinyl dimethoxysilane and an acrylate monomer, and reacting at 90-95 ℃ for 2-3h to obtain the low-VOC aqueous epoxy emulsion.
The invention has the following beneficial effects:
the epoxy resin, the methyl vinyl dimethoxysilane and the acrylate monomer are subjected to ring-opening grafting under the action of the reactive emulsifier and the initiator, so that the stability, the water resistance and the flexibility of the water-based epoxy emulsion are improved.
The reactive emulsifier selected by the invention is prepared from epoxy resin, maleic acid mono-polyethylene glycol monomethyl ether ester and an alkaline catalyst, has good emulsifying property, and can further improve the stability and water resistance of the aqueous epoxy resin emulsion.
The preparation process of the invention does not contain organic volatile matters, is environment-friendly and pollution-free, and the prepared waterborne epoxy emulsion has low viscosity, small particle size, good dispersibility and stability, no delamination, no sedimentation and no flocculation after being stored for 1 month at 50 ℃, no delamination, no sedimentation, no flocculation and no obvious change in viscosity after being stored for 8 months at normal temperature.
Detailed Description
The present invention will be described in detail with reference to examples, which are only preferred embodiments of the present invention and are not intended to limit the present invention.
The following table shows the formulation (unit:%) of 3 examples of the low VOC aqueous epoxy emulsion of the present invention.
| Components | Example 1 | Example 2 | Example 3 |
| Epoxy resin | Phenol-aralkyl type epoxy resin, 35% | Phenol-aralkyl type epoxy resin, 40% | 45 percent of trisphenol methane type epoxy resin |
| Methyl vinyl dimethoxy silane | 1 | 1.5 | 2 |
| Initiator | Ammonium persulfate, 0.1% | 0.8 percent of potassium persulfate | Sodium persulfate, 1.2% |
| Reactive emulsifier | 0.5 | 1.2 | 2 |
| Acrylic ester monomer | Methyl acrylate, 3% | Butyl methacrylate, 4% | Isooctyl methacrylate, 5% |
| Epoxy diluent | Octyl glycidyl ether, 2% | Trimethylolpropane triglycidyl ether, 2.8% | TrimethylolpropaneTriglycidyl ether, 3.5% |
| Water (W) | 58.4 | 49.7 | 41.3。 |
The following table shows the formulation of the reactive emulsifier used in 3 examples of the low VOC aqueous epoxy emulsion of the present invention (unit:%).
| Components | Example 1 | Example 2 | Example 3 |
| Epoxy resin | Phenol-aralkyl type epoxy resin, 25% | Phenol-aralkyl type epoxy resin, 32% | Trisphenol methane type epoxy resin, 40% |
| Maleic acid mono-polyethylene glycol monomethyl ether ester | 74 | 66.5 | 58 |
| Basic catalyst | 1 | 1.5 | 2。 |
The preparation method of the low-VOC aqueous epoxy emulsion comprises the following steps:
s1, mixing epoxy resin, maleic acid mono-polyethylene glycol monomethyl ether ester and an alkaline catalyst, and reacting at the temperature of 180 ℃ and 220 ℃ for 5-8h to obtain a reactive emulsifier;
s2, uniformly mixing an initiator, a reactive emulsifier and water, adding epoxy resin, an epoxy diluent, methyl vinyl dimethoxysilane and an acrylate monomer, and reacting at 90-95 ℃ for 2-3h to obtain the low-VOC aqueous epoxy emulsion
The performances of 3 embodiments of the low VOC aqueous epoxy emulsion of the invention were tested, and the test items and results are shown in the following table.
| Item | Standard of merit | Example 1 | Example 2 | Example 3 |
| Appearance of the product | / | Milky white liquid | Milky white liquid | Milky white liquid |
| Particle size/. mu.m | / | 1.2 | 1.2 | 1.3 |
| viscosity/mPa. cndot s | GB/T2794 | 400-1000 | 400-1200 | 500-1500 |
| Solids content/% | GB/T6751-1986 | 52±1 | 53±1 | 55±1 |
| Calcium ion stabilization Property of (2) | 48h,5% NaCl solution Liquid for treating urinary tract infection | No layering, no precipitation and no flocculation | No layering, no precipitation and no flocculation | No layering, no precipitation and no flocculation |
| Mechanical stability | 3000r/min, 30min | No layering, no precipitation and no flocculation | No layering, no precipitation and no flocculation | No layering, no precipitation and no flocculation |
| Stability in dilution | 72, 3% concentration | No layering, no precipitation and no flocculation | No layering, no precipitation and no flocculation | No layering, no precipitation and no flocculation |
| Thermal stability | Heat storage at 50 deg.C for 30d | No layering, no precipitation and no flocculation | No layering, no precipitation and no flocculation | No layering, no precipitation and no flocculation |
| Stability of | Normal temperature storage 240d | No demixing, no precipitation, no flocculation and no obvious viscosity Variations in | No demixing, no precipitation, no flocculation and no obvious viscosity Variations in | No demixing, no precipitation, no flocculation and no obvious viscosity And (4) changing. |
Therefore, the calcium ion-containing nano-particles have the advantages of low viscosity, small particle size, and good calcium ion stability, mechanical stability, dilution stability and thermal stability.
The water-based epoxy emulsion disclosed by the invention is low in viscosity, small in particle size, good in dispersity, stability, water resistance and flexibility, free of organic volatile matters, environment-friendly and pollution-free.
Claims (7)
1. The low-VOC aqueous epoxy emulsion is characterized by being prepared from the following components in percentage by weight:
35 to 45 percent of epoxy resin,
1 to 2 percent of methyl vinyl dimethoxy silane,
0.1 to 1.2 percent of initiator,
0.5 to 2 percent of reactive emulsifier,
3 to 5 percent of acrylate monomer,
2 to 3.5 percent of epoxy diluent,
40-60% of water;
the reactive emulsifier is prepared from the following components in percentage by weight:
25 to 40 percent of epoxy resin,
58-74 percent of maleic acid mono-polyethylene glycol mono-methyl ether ester,
1-2% of alkaline catalyst.
2. The low VOC aqueous epoxy emulsion of claim 1 wherein said epoxy resins are phenol-aralkyl type epoxy resins and triphenolmethane type epoxy resins.
3. The low VOC aqueous epoxy emulsion of claim 1 wherein said initiator is one of ammonium persulfate, potassium persulfate, and sodium persulfate.
4. The low VOC aqueous epoxy emulsion of claim 1 wherein said acrylate monomer is at least one of methyl acrylate, butyl methacrylate, ethyl acrylate or isooctyl methacrylate.
5. The low VOC aqueous epoxy emulsion of claim 1 wherein said epoxy diluent is octyl glycidyl ether or trimethylolpropane triglycidyl ether.
6. The low VOC aqueous epoxy emulsion of claim 1 wherein said basic catalyst is at least one of N, N-dimethylbenzylamine, triethanolamine salt, 2-methyl-3 imidazole, and N, N-dimethylethanolamine, tetramethylammonium bromide, tetramethylammonium chloride, tetraethylammonium bromide, tetraethylammonium chloride, tetrabutylammonium chloride, benzyltriethylammonium chloride, and hexadecyltrimethylammonium bromide.
7. A method of preparing the low VOC aqueous epoxy emulsion of any of claims 1-6 comprising the steps of:
s1, mixing epoxy resin, maleic acid mono-polyethylene glycol monomethyl ether ester and an alkaline catalyst, and reacting at the temperature of 180 ℃ and 220 ℃ for 5-8h to obtain a reactive emulsifier;
s2, uniformly mixing an initiator, a reactive emulsifier and water, adding epoxy resin, an epoxy diluent, methyl vinyl dimethoxysilane and an acrylate monomer, and reacting at 90-95 ℃ for 2-3h to obtain the low-VOC aqueous epoxy emulsion.
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| CN201911179641.7A CN110776605B (en) | 2019-11-27 | 2019-11-27 | Low-VOC (volatile organic compound) water-based epoxy emulsion and preparation method thereof |
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| CN201911179641.7A CN110776605B (en) | 2019-11-27 | 2019-11-27 | Low-VOC (volatile organic compound) water-based epoxy emulsion and preparation method thereof |
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| CN110776605B true CN110776605B (en) | 2021-12-31 |
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Citations (5)
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|---|---|---|---|---|
| CN102153934A (en) * | 2011-01-26 | 2011-08-17 | 合肥工业大学 | Aqueous oil polish and preparation method thereof |
| CN102399309A (en) * | 2010-09-10 | 2012-04-04 | 宏峰行化工(深圳)有限公司 | Novel reactive emulsifier and its preparation method |
| CN105084844A (en) * | 2015-08-31 | 2015-11-25 | 武汉理工大学 | Epoxy resin emulsion modified cement-based patching material and preparation material thereof |
| CN107603410A (en) * | 2017-10-13 | 2018-01-19 | 武汉工程大学 | Floor coatings aqueous epoxy resin emulsion and preparation method thereof |
| CN108329438A (en) * | 2018-02-26 | 2018-07-27 | 华南理工大学 | High-acid-resistance water-based epoxy dispersion and preparation method thereof |
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- 2019-11-27 CN CN201911179641.7A patent/CN110776605B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102399309A (en) * | 2010-09-10 | 2012-04-04 | 宏峰行化工(深圳)有限公司 | Novel reactive emulsifier and its preparation method |
| CN102153934A (en) * | 2011-01-26 | 2011-08-17 | 合肥工业大学 | Aqueous oil polish and preparation method thereof |
| CN105084844A (en) * | 2015-08-31 | 2015-11-25 | 武汉理工大学 | Epoxy resin emulsion modified cement-based patching material and preparation material thereof |
| CN107603410A (en) * | 2017-10-13 | 2018-01-19 | 武汉工程大学 | Floor coatings aqueous epoxy resin emulsion and preparation method thereof |
| CN108329438A (en) * | 2018-02-26 | 2018-07-27 | 华南理工大学 | High-acid-resistance water-based epoxy dispersion and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 水性环氧树脂乳液的制备及其应用;李晴等;《涂料工业》;20150301(第03期);第41-45页 * |
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