CN108285525B - Method for preparing epoxy resin emulsifier and water-based epoxy resin - Google Patents
Method for preparing epoxy resin emulsifier and water-based epoxy resin Download PDFInfo
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- CN108285525B CN108285525B CN201810134467.3A CN201810134467A CN108285525B CN 108285525 B CN108285525 B CN 108285525B CN 201810134467 A CN201810134467 A CN 201810134467A CN 108285525 B CN108285525 B CN 108285525B
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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
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
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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
- C08G59/62—Alcohols or phenols
- C08G59/64—Amino alcohols
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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
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
- C08L95/005—Aqueous compositions, e.g. emulsions
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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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Emergency Medicine (AREA)
- Engineering & Computer Science (AREA)
- Civil Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Epoxy Resins (AREA)
- Paints Or Removers (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention provides a method for preparing an epoxy resin emulsifier, which comprises the following steps: mixing the component A and the component B and uniformly stirring to obtain an epoxy resin emulsifier; wherein the mass part ratio of the component A to the component B is 1: 1; in the component A, the mass part ratio of epoxy resin E-51, ethylene glycol monobutyl ether, diethanolamine and bromoethane is 100: 40: 54: 54, a first electrode; in the component B, the mass part ratio of epoxy resin E-51, polyethylene glycol 600 and N, N-dimethylethanolamine is 100: 306: 6. the beneficial technical effects of the invention are as follows: the invention provides a method for preparing an epoxy resin emulsifier and water-based epoxy resin, and the technical conditions only need a 90-120 ℃ closed environment when the epoxy resin emulsifier is prepared by adopting the scheme of the invention, so that the method is simple and easy to popularize.
Description
Technical Field
The invention relates to a preparation technology of an epoxy resin emulsifier, in particular to a method for preparing an epoxy resin emulsifier and water-based epoxy resin.
Background
The highway in China gradually enters a maintenance period from a large construction period, and the micro-surfacing is widely applied to road maintenance as an economic, effective, rapid and environment-friendly maintenance mode. However, the micro-surfacing overlay is thin and is positioned on the surface layer of the pavement, and is directly and repeatedly acted by natural conditions and vehicle loads, so that the requirement on the performance of the mixture is high, and the expected use effect is often difficult to achieve in practice.
The water-based epoxy resin system can be cured at room temperature and in a humid environment, has reasonable curing time, can ensure high crosslinking density, and is widely applied to the fields of high-cleanness industrial places, indoor coating, high-impermeability waterproof coatings, anticorrosive coatings of wooden furniture, floors and metal materials and the like.
The aqueous epoxy modified emulsified asphalt is modified by means of the characteristics of high viscosity, chemical stability, high strength and the like of an epoxy resin cured structure, so that various road performances of high-temperature stability, rutting resistance, wear resistance and the like of an asphalt mixture are improved. The modified emulsified asphalt produced by the existing waterborne epoxy system in the market still has the defects of poor bonding property with the old pavement, low crack resistance and the like in practical application, so that the waterborne epoxy system is further researched, and various properties of the waterborne epoxy modified emulsified asphalt in a micro-surfacing asphalt mixture are improved, so that the requirement of highway maintenance is met.
Disclosure of Invention
Aiming at the problems in the background art, the invention provides a method for preparing an epoxy resin emulsifier, which is innovative in that: the method comprises the following steps: mixing the component A and the component B and uniformly stirring to obtain an epoxy resin emulsifier; wherein the mass part ratio of the component A to the component B is 1: 1;
component a was prepared as follows:
1) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding ethylene glycol monobutyl ether into the epoxy resin E-51 and stirring until the epoxy resin E-51 is dissolved to obtain a product C; ethylene glycol monobutyl ether plays a role of a solvent and introduces ether functional groups;
2) adding diethanolamine into the product C and uniformly stirring to obtain a product D; in the process, an epoxy group in the epoxy resin E-51 and diethanol amine generate ring-opening addition reaction to generate a tertiary amino structure intermediate;
3) under the condition of air isolation, heating the product D to 90-100 ℃, reacting for 4 hours, then adding bromoethane, stirring uniformly, and continuing to react for 50 minutes to obtain a product E; in this process, tertiary amine groups are converted to quaternary ammonium salts by bromoethane;
3) under the condition of air isolation, cooling the product E to 45 ℃, and adding water to adjust the solid content to 50% to obtain a component A;
component B was prepared as follows:
a) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding polyethylene glycol 600 and N, N-dimethylethanolamine into the epoxy resin E-51 to obtain a product F; in the process, an epoxy group in the epoxy resin E-51 and polyethylene glycol 600 undergo a ring-opening addition reaction; n, N-dimethylethanolamine as a catalyst;
b) under the condition of air isolation, heating the product F to 110-120 ℃, and reacting for 1h to obtain a product G;
c) under the condition of air isolation, cooling the product G to 45 ℃, adding water to adjust the solid content to 50%, and then standing until bubbles disappear to obtain a component B;
in the component A, the mass part ratio of epoxy resin E-51, ethylene glycol monobutyl ether, diethanolamine and bromoethane is 100: 40: 54: 54, a first electrode;
in the component B, the mass part ratio of epoxy resin E-51, polyethylene glycol 600 and N, N-dimethylethanolamine is 100: 306: 6.
based on the epoxy resin emulsifier obtained by the scheme, the invention also provides a method for preparing the water-based epoxy resin, which is innovative in that: the method comprises the following steps:
(1) adding 100 parts of epoxy resin E-51 and 25 parts of epoxy resin emulsifier into a reaction kettle, and uniformly stirring at a rotating speed of 800-1000 r/min by using a sand grinding stirring dispersion machine to obtain a product H;
(2) adding 100 parts of deionized water at 50 ℃ into the product H for multiple times at intervals of 15-20 s, wherein the added deionized water is not more than 12 parts each time, and stirring the product H in the process of adding the deionized water; finally obtaining the water-based epoxy resin;
the preparation method of the waterborne epoxy resin is as described above;
the beneficial technical effects of the invention are as follows: the invention provides a method for preparing an epoxy resin emulsifier and water-based epoxy resin, and the technical conditions only need a 90-120 ℃ closed environment when the epoxy resin emulsifier is prepared by adopting the scheme of the invention, so that the method is simple and easy to popularize.
Detailed Description
The method for preparing the epoxy resin emulsifier is characterized by comprising the following steps: the method comprises the following steps: mixing the component A and the component B and uniformly stirring to obtain an epoxy resin emulsifier; wherein the mass part ratio of the component A to the component B is 1: 1;
component a was prepared as follows:
1) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding ethylene glycol monobutyl ether into the epoxy resin E-51 and stirring until the epoxy resin E-51 is dissolved to obtain a product C;
2) adding diethanolamine into the product C and uniformly stirring to obtain a product D;
3) under the condition of air isolation, heating the product D to 90-100 ℃, reacting for 4 hours, then adding bromoethane, stirring uniformly, and continuing to react for 50 minutes to obtain a product E;
3) under the condition of air isolation, cooling the product E to 45 ℃, and adding water to adjust the solid content to 50% to obtain a component A;
component B was prepared as follows:
a) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding polyethylene glycol 600 and N, N-dimethylethanolamine into the epoxy resin E-51 to obtain a product F;
b) under the condition of air isolation, heating the product F to 110-120 ℃, and reacting for 1h to obtain a product G;
c) under the condition of air isolation, cooling the product G to 45 ℃, adding water to adjust the solid content to 50%, and then standing until bubbles disappear to obtain a component B;
in the component A, the mass part ratio of epoxy resin E-51, ethylene glycol monobutyl ether, diethanolamine and bromoethane is 100: 40: 54: 54, a first electrode;
in the component B, the mass part ratio of epoxy resin E-51, polyethylene glycol 600 and N, N-dimethylethanolamine is 100: 306: 6.
the innovation of the method for preparing the water-based epoxy resin is as follows: the method comprises the following steps:
(1) adding 100 parts of epoxy resin E-51 and 25 parts of epoxy resin emulsifier into a reaction kettle, and uniformly stirring at a rotating speed of 800-1000 r/min by using a sand grinding stirring dispersion machine to obtain a product H;
(2) adding 100 parts of deionized water at 50 ℃ into the product H for multiple times at intervals of 15-20 s, wherein the added deionized water is not more than 12 parts each time, and stirring the product H in the process of adding the deionized water; finally obtaining the water-based epoxy resin;
the preparation method of the water-based epoxy resin comprises the following steps: mixing the component A and the component B and uniformly stirring to obtain an epoxy resin emulsifier; wherein the mass part ratio of the component A to the component B is 1: 1;
component a was prepared as follows:
1) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding ethylene glycol monobutyl ether into the epoxy resin E-51 and stirring until the epoxy resin E-51 is dissolved to obtain a product C;
2) adding diethanolamine into the product C and uniformly stirring to obtain a product D;
3) under the condition of air isolation, heating the product D to 90-100 ℃, reacting for 4 hours, then adding bromoethane, stirring uniformly, and continuing to react for 50 minutes to obtain a product E;
3) under the condition of air isolation, cooling the product E to 45 ℃, and adding water to adjust the solid content to 50% to obtain a component A;
component B was prepared as follows:
a) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding polyethylene glycol 600 and N, N-dimethylethanolamine into the epoxy resin E-51 to obtain a product F;
b) under the condition of air isolation, heating the product F to 110-120 ℃, and reacting for 1h to obtain a product G;
c) under the condition of air isolation, cooling the product G to 45 ℃, adding water to adjust the solid content to 50%, and then standing until bubbles disappear to obtain a component B;
in the component A, the mass part ratio of epoxy resin E-51, ethylene glycol monobutyl ether, diethanolamine and bromoethane is 100: 40: 54: 54, a first electrode;
in the component B, the mass part ratio of epoxy resin E-51, polyethylene glycol 600 and N, N-dimethylethanolamine is 100: 306: 6.
the epoxy resin emulsifier contains the following five substances;
substance 1:
substance 2:
substance 3:
substance 4:
substance 5:
wherein R represents the following group:
wherein, the substance 1, the substance 3 and the substance 4 are quaternary ammonium salt cationic surfactants;
after the component A and the component B are prepared according to the scheme of the invention, in order to determine the proportion of the component A and the component B, the inventor respectively adopts a plurality of proportions to prepare the epoxy resin emulsifier, and then a standing layering test is carried out, and the test results are shown in Table 1:
TABLE 1
| Serial number | A︰B | Standing and layering time/h |
| 1 | 0:100 | 10 |
| 2 | 10:90 | 24 |
| 3 | 20:80 | 72 |
| 4 | 30:70 | 120 |
| 5 | 40:60 | 264 |
| 6 | 50:50 | >480 |
| 7 | 60:40 | 480 |
| 8 | 70:30 | 168 |
| 9 | 80:20 | 120 |
| 10 | 90:10 | 48 |
| 11 | 100:0 | 10 |
As can be seen from Table 1, when the ratio of component A to component B is 1: 1, the standing and layering time of the epoxy resin emulsifier is longest, so that the ratio of component A to component B is 1: 1;
when preparation waterborne epoxy, the sanding stirring dispenser adopts different rotational speeds to make many batches of samples, carries out the layering test that stews, and the test result is shown in table 2:
TABLE 2
As can be seen from Table 2, when the rotation speed is 800-1000 r/min, the standing and layering time of the waterborne epoxy resin is longest, so that the rotation speed is determined to be 800-1000 r/min.
Through determination, the rotational viscosity of the water-based epoxy resin disclosed by the invention is mutated when the solid content is 50%, and is a phase transition point, an epoxy resin aqueous solution is formed, and the proportion of deionized water and the water-based epoxy resin is determined.
Changing the dosage of the epoxy resin emulsifier, keeping other conditions unchanged, and observing the standing and layering time of the emulsion, wherein the observation result shows that the standing and layering time of the emulsion is more than 480h when the dosage of the emulsifier is 20%, and the effect is equivalent to that when the dosage of the emulsifier is 20% when the dosage of the emulsifier is 25%, so that the dosage of 20% is taken as the optimal emulsifier dosage.
When the water-based epoxy modified emulsified asphalt is used specifically, the matrix emulsified asphalt and the water-based epoxy curing system are firstly prepared, and then 92 parts of the matrix emulsified asphalt and 8 parts of the water-based epoxy curing system are mixed and stirred uniformly to prepare the water-based epoxy modified emulsified asphalt; wherein the formula of the matrix emulsified asphalt is 90#60 parts of matrix asphalt, 2 parts of asphalt emulsifier (cationic emulsifier), 0.1 part of stabilizer (calcium chloride), 1 part of hydrochloric acid and 37 parts of water, and the substances are uniformly mixed to obtain matrix emulsified asphalt; the waterborne epoxy curing system is prepared by the waterborne epoxy resin, and is prepared by mixing the waterborne epoxy resin with an amine curing agent, wherein the specific ratio of the waterborne epoxy resin to the amine curing agent is determined by the ratio of epoxy groups in the waterborne epoxy resin to active hydrogen atoms in the amine curing agent being 1: 1.
Claims (2)
1. A method for preparing an epoxy resin emulsifier is characterized by comprising the following steps: the method comprises the following steps: mixing the component A and the component B and uniformly stirring to obtain an epoxy resin emulsifier; wherein the mass part ratio of the component A to the component B is 1: 1;
component a was prepared as follows:
1) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding ethylene glycol monobutyl ether into the epoxy resin E-51 and stirring until the epoxy resin E-51 is dissolved to obtain a product C;
2) adding diethanolamine into the product C and uniformly stirring to obtain a product D;
3) under the condition of air isolation, heating the product D to 90-100 ℃, reacting for 4 hours, then adding bromoethane, stirring uniformly, and continuing to react for 50 minutes to obtain a product E;
4) under the condition of air isolation, cooling the product E to 45 ℃, and adding water to adjust the solid content to 50% to obtain a component A;
component B was prepared as follows:
a) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding polyethylene glycol 600 and N, N-dimethylethanolamine into the epoxy resin E-51 to obtain a product F;
b) under the condition of air isolation, heating the product F to 110-120 ℃, and reacting for 1h to obtain a product G;
c) under the condition of air isolation, cooling the product G to 45 ℃, adding water to adjust the solid content to 50%, and then standing until bubbles disappear to obtain a component B;
in the component A, the mass part ratio of epoxy resin E-51, ethylene glycol monobutyl ether, diethanolamine and bromoethane is 100: 40: 54: 54, a first electrode;
in the component B, the mass part ratio of epoxy resin E-51, polyethylene glycol 600 and N, N-dimethylethanolamine is 100: 306: 6.
2. a method of making a waterborne epoxy resin, comprising: the method comprises the following steps:
(1) adding 100 parts of epoxy resin E-51 and 25 parts of epoxy resin emulsifier into a reaction kettle, and uniformly stirring at a rotating speed of 800-1000 r/min by using a sand grinding stirring dispersion machine to obtain a product H;
(2) adding 100 parts of deionized water at 50 ℃ into the product H for multiple times at intervals of 15-20 s, wherein the added deionized water is not more than 12 parts each time, and stirring the product H in the process of adding the deionized water; finally obtaining the water-based epoxy resin;
the preparation method of the epoxy resin emulsifier comprises the following steps: mixing the component A and the component B and uniformly stirring to obtain an epoxy resin emulsifier; wherein the mass part ratio of the component A to the component B is 1: 1;
component a was prepared as follows:
1) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding ethylene glycol monobutyl ether into the epoxy resin E-51 and stirring until the epoxy resin E-51 is dissolved to obtain a product C;
2) adding diethanolamine into the product C and uniformly stirring to obtain a product D;
3) under the condition of air isolation, heating the product D to 90-100 ℃, reacting for 4 hours, then adding bromoethane, stirring uniformly, and continuing to react for 50 minutes to obtain a product E;
4) Under the condition of air isolation, cooling the product E to 45 ℃, and adding water to adjust the solid content to 50% to obtain a component A;
component B was prepared as follows:
a) preheating and softening the epoxy resin E-51 for 1 hour at the temperature of 50 ℃; then adding polyethylene glycol 600 and N, N-dimethylethanolamine into the epoxy resin E-51 to obtain a product F;
b) under the condition of air isolation, heating the product F to 110-120 ℃, and reacting for 1h to obtain a product G;
c) under the condition of air isolation, cooling the product G to 45 ℃, adding water to adjust the solid content to 50%, and then standing until bubbles disappear to obtain a component B;
in the component A, the mass part ratio of epoxy resin E-51, ethylene glycol monobutyl ether, diethanolamine and bromoethane is 100: 40: 54: 54, a first electrode;
in the component B, the mass part ratio of epoxy resin E-51, polyethylene glycol 600 and N, N-dimethylethanolamine is 100: 306: 6.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101117377A (en) * | 2007-09-18 | 2008-02-06 | 天津大学 | Method for preparing aqueous epoxy resin |
| CN103497338A (en) * | 2013-07-29 | 2014-01-08 | 中国石油大学(华东) | Preparation and application method of ionic emulsifier special for epoxy resin in waterborne epoxy coating |
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2018
- 2018-02-09 CN CN201810134467.3A patent/CN108285525B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101117377A (en) * | 2007-09-18 | 2008-02-06 | 天津大学 | Method for preparing aqueous epoxy resin |
| CN103497338A (en) * | 2013-07-29 | 2014-01-08 | 中国石油大学(华东) | Preparation and application method of ionic emulsifier special for epoxy resin in waterborne epoxy coating |
Non-Patent Citations (1)
| Title |
|---|
| "水性环氧树脂专用乳化剂的制备及性能研究";倪维良等;《涂料工业》;20101231;第40卷(第12期);第61-64页 * |
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Application publication date: 20180717 Assignee: Guizhou kunzhibao New Material Co., Ltd Assignor: CHONGQING JIAOTONG University Contract record no.: X2020990000557 Denomination of invention: Preparation of epoxy emulsifier and waterborne epoxy resin Granted publication date: 20200616 License type: Common License Record date: 20201023 |
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