CN105315436A - Polyether type epoxy resin curing agent and preparation method thereof - Google Patents
Polyether type epoxy resin curing agent and preparation method thereof Download PDFInfo
- Publication number
- CN105315436A CN105315436A CN201510691984.7A CN201510691984A CN105315436A CN 105315436 A CN105315436 A CN 105315436A CN 201510691984 A CN201510691984 A CN 201510691984A CN 105315436 A CN105315436 A CN 105315436A
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- epoxy resin
- reaction
- polyether
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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
Abstract
The invention relates to a polyether type epoxy resin curing agent and a preparation method thereof and belongs to the technical field of curing agents. The polyether type epoxy resin curing agent is prepared from, by weight, 20-30 parts of polyether, 20-30 parts of epoxy resin, 15-25 parts of SXH-152, 0.5-2.5 parts of boron trifluoride, 30-40 parts of methylbenzene, 10-20 parts of polyethylene polyamine, 10-20 parts of single-epoxy compounds and 5-15 parts of glacial acetic acid. The defects are overcome through the method of introducing a polyether chain segment in the curing agent. Polyethylene polyamine, liquid epoxy resin and SXH-152 modified polyether are used for reacting, and an ABA type amino-terminated epoxy-amine addition product is synthesized. Then through the process of epoxy-amine addition, single epoxy end sealing and acidification salifying, the epoxy resin curing agent is synthesized, and the flexibility and impact resistance of the polyether type epoxy resin curing agent are improved.
Description
Technical field
The present invention relates to a kind of solidifying agent and preparation method thereof, more particularly, the present invention relates to a kind of polyether-type epoxy resin solidifying agent and preparation method thereof, belong to solidifying agent technical field.
Background technology
Epoxy coating excellent property, is widely used in the field such as anticorrosion, industry ground slab, building.But the epoxy coating used at present is mainly solvent based coating, in recent years, along with improving constantly of people's environmental consciousness, many countries have promulgated the environmental regulation of restriction volatile organic solvent (VOC) in succession, and the differentiation of the Water-borne modification of coating, solvent free and high solid has become the inexorable trend of paint development.
Aqueous epoxy resin systems has become the emphasis of resin industry research, and as the necessary component of aqueous epoxy resin systems, the research and development of aqueous epoxy curing agent are also increasingly important.Solidifying agent is one of key factor affecting bi-component epoxy coating property, and the actual aqueous epoxy curing agent used is mostly their modified product at present, comprises amidation polyamines and epoxy one polyamines affixture.
Due to the water tolerance of film after the solidification of amides solidifying agent and chemical proofing poor, the epoxy one polyamines class affixture of the aqueous epoxy curing agent of research now mainly end-blocking.The hardness of the film of common aqueous epoxide resin paint is higher, but snappiness and shock resistance are all poor.
Summary of the invention
The present invention is intended to solve existing epoxy curing agent film snappiness and all poor problem of shock resistance, and provide a kind of polyether-type epoxy resin solidifying agent, not only hardness is high for this epoxy curing agent film, and has preferably snappiness and shock resistance.
In order to realize foregoing invention object, its concrete technical scheme is as follows:
A kind of polyether-type epoxy resin solidifying agent, is characterized in that: comprise the following raw material according to weight parts:
Polyethers 20-30 part
Epoxy resin 20-30 part
SXH-15215-25 part
Boron trifluoride 0.5-2.5 part
Toluene 30-40 part
Polyethylene polyamine 10-20 part
Mono-epoxy compounds 10-20 part
Glacial acetic acid 5-15 part.
Epoxy resin of the present invention is epoxy resin E-42.
A preparation method for polyether-type epoxy resin solidifying agent, is characterized in that: comprise following processing step:
A, polyethers and SXH-152 are added in flask, start and be uniformly mixed; Logical nitrogen, heating, stirs and makes it to mix further; The boron trifluoride being dissolved in toluene is in advance placed in constant pressure funnel, slowly drips the toluene solution of boron trifluoride;
B, between temperature 40-60 DEG C maintain reaction 4-6h; Underpressure distillation desolventizing, discharging obtains polyethers synthetics, for subsequent use;
C, get polyethers synthetics, epoxy resin, polyethylene polyamine that step B obtains, be placed in four-hole boiling flask; Temperature of reaction is risen to 80 DEG C, reaction 2-4h; Temperature of reaction is risen to 90 DEG C, reaction 2-4h; Underpressure distillation, removes unnecessary polyethylene polyamine; Add mono-epoxy compounds after being down to room temperature, maintain temperature of reaction 60 DEG C, reaction 4-6h;
D, add Glacial acetic acid, maintain temperature of reaction 40 DEG C, reaction 4-6h, obtains polyether-type epoxy resin solidifying agent.
The Advantageous Effects that the present invention brings:
The invention solves existing epoxy curing agent film snappiness and all poor problem of shock resistance.The present invention adopts the method introducing polyether segment in solidifying agent to improve these shortcomings.React with polyethylene polyamine, liquid epoxies and SXH-152 modified polyether, synthesis ABA type Amino End Group epoxy one amine additives.Then by the addition of epoxy one amine, single epoxy-capped, the technique of acidifying salify, synthetic epoxy resin solidifying agent, improves its snappiness and shock resistance.
Embodiment
embodiment 1
A kind of polyether-type epoxy resin solidifying agent, comprises the following raw material according to weight parts:
Polyethers 20 parts
Epoxy resin 20 parts
SXH-15215 part
Boron trifluoride 0.5 part
Toluene 30 parts
Polyethylene polyamine 10 parts
Mono-epoxy compounds 10 parts
5 parts, Glacial acetic acid.
embodiment 2
A kind of polyether-type epoxy resin solidifying agent, comprises the following raw material according to weight parts:
Polyethers 30 parts
Epoxy resin 30 parts
SXH-15225 part
Boron trifluoride 2.5 parts
Toluene 40 parts
Polyethylene polyamine 20 parts
Mono-epoxy compounds 20 parts
15 parts, Glacial acetic acid.
embodiment 3
A kind of polyether-type epoxy resin solidifying agent, comprises the following raw material according to weight parts:
Polyethers 25 parts
Epoxy resin 25 parts
SXH-15220 part
Boron trifluoride 1.5 parts
Toluene 35 parts
Polyethylene polyamine 15 parts
Mono-epoxy compounds 15 parts
10 parts, Glacial acetic acid.
embodiment 4
A kind of polyether-type epoxy resin solidifying agent, comprises the following raw material according to weight parts:
Polyethers 21 parts
Epoxy resin 21 parts
SXH-15222 part
Boron trifluoride 2 parts
Toluene 38 parts
Polyethylene polyamine 16 parts
Mono-epoxy compounds 11 parts
13 parts, Glacial acetic acid.
embodiment 5
A preparation method for polyether-type epoxy resin solidifying agent, comprises following processing step:
A, polyethers and SXH-152 are added in flask, start and be uniformly mixed; Logical nitrogen, heating, stirs and makes it to mix further; The boron trifluoride being dissolved in toluene is in advance placed in constant pressure funnel, slowly drips the toluene solution of boron trifluoride;
B, between temperature 40 DEG C maintain reaction 4h; Underpressure distillation desolventizing, discharging obtains polyethers synthetics, for subsequent use;
C, get polyethers synthetics, epoxy resin, polyethylene polyamine that step B obtains, be placed in four-hole boiling flask; Temperature of reaction is risen to 80 DEG C, reaction 2h; Temperature of reaction is risen to 90 DEG C, reaction 2h; Underpressure distillation, removes unnecessary polyethylene polyamine; Add mono-epoxy compounds after being down to room temperature, maintain temperature of reaction 60 DEG C, reaction 4h;
D, add Glacial acetic acid, maintain temperature of reaction 40 DEG C, reaction 4h, obtains polyether-type epoxy resin solidifying agent.
embodiment 6
A preparation method for polyether-type epoxy resin solidifying agent, comprises following processing step:
A, polyethers and SXH-152 are added in flask, start and be uniformly mixed; Logical nitrogen, heating, stirs and makes it to mix further; The boron trifluoride being dissolved in toluene is in advance placed in constant pressure funnel, slowly drips the toluene solution of boron trifluoride;
B, between temperature 60 C maintain reaction 6h; Underpressure distillation desolventizing, discharging obtains polyethers synthetics, for subsequent use;
C, get polyethers synthetics, epoxy resin, polyethylene polyamine that step B obtains, be placed in four-hole boiling flask; Temperature of reaction is risen to 80 DEG C, reaction 4h; Temperature of reaction is risen to 90 DEG C, reaction 4h; Underpressure distillation, removes unnecessary polyethylene polyamine; Add mono-epoxy compounds after being down to room temperature, maintain temperature of reaction 60 DEG C, reaction 6h;
D, add Glacial acetic acid, maintain temperature of reaction 40 DEG C, reaction 6h, obtains polyether-type epoxy resin solidifying agent.
embodiment 7
A preparation method for polyether-type epoxy resin solidifying agent, comprises following processing step:
A, polyethers and SXH-152 are added in flask, start and be uniformly mixed; Logical nitrogen, heating, stirs and makes it to mix further; The boron trifluoride being dissolved in toluene is in advance placed in constant pressure funnel, slowly drips the toluene solution of boron trifluoride;
B, between temperature 50 C maintain reaction 5h; Underpressure distillation desolventizing, discharging obtains polyethers synthetics, for subsequent use;
C, get polyethers synthetics, epoxy resin, polyethylene polyamine that step B obtains, be placed in four-hole boiling flask; Temperature of reaction is risen to 80 DEG C, reaction 3h; Temperature of reaction is risen to 90 DEG C, reaction 3h; Underpressure distillation, removes unnecessary polyethylene polyamine; Add mono-epoxy compounds after being down to room temperature, maintain temperature of reaction 60 DEG C, reaction 5h;
D, add Glacial acetic acid, maintain temperature of reaction 40 DEG C, reaction 5h, obtains polyether-type epoxy resin solidifying agent.
embodiment 8
A preparation method for polyether-type epoxy resin solidifying agent, comprises following processing step:
A, polyethers and SXH-152 are added in flask, start and be uniformly mixed; Logical nitrogen, heating, stirs and makes it to mix further; The boron trifluoride being dissolved in toluene is in advance placed in constant pressure funnel, slowly drips the toluene solution of boron trifluoride;
B, between temperature 42 DEG C maintain reaction 5.5h; Underpressure distillation desolventizing, discharging obtains polyethers synthetics, for subsequent use;
C, get polyethers synthetics, epoxy resin, polyethylene polyamine that step B obtains, be placed in four-hole boiling flask; Temperature of reaction is risen to 80 DEG C, reaction 3.5h; Temperature of reaction is risen to 90 DEG C, reaction 2.5h; Underpressure distillation, removes unnecessary polyethylene polyamine; Add mono-epoxy compounds after being down to room temperature, maintain temperature of reaction 60 DEG C, reaction 5.5h;
D, add Glacial acetic acid, maintain temperature of reaction 40 DEG C, reaction 5.5h, obtains polyether-type epoxy resin solidifying agent.
Claims (3)
1. a polyether-type epoxy resin solidifying agent, is characterized in that: comprise the following raw material according to weight parts:
Polyethers 20-30 part
Epoxy resin 20-30 part
SXH-15215-25 part
Boron trifluoride 0.5-2.5 part
Toluene 30-40 part
Polyethylene polyamine 10-20 part
Mono-epoxy compounds 10-20 part
Glacial acetic acid 5-15 part.
2. a kind of polyether-type epoxy resin solidifying agent according to claim 1, is characterized in that: described epoxy resin is epoxy resin E-42.
3. the preparation method of a kind of polyether-type epoxy resin solidifying agent according to claim 1, is characterized in that: comprise following processing step:
A, polyethers and SXH-152 are added in flask, start and be uniformly mixed; Logical nitrogen, heating, stirs and makes it to mix further; The boron trifluoride being dissolved in toluene is in advance placed in constant pressure funnel, slowly drips the toluene solution of boron trifluoride;
B, between temperature 40-60 DEG C maintain reaction 4-6h; Underpressure distillation desolventizing, discharging obtains polyethers synthetics, for subsequent use;
C, get polyethers synthetics, epoxy resin, polyethylene polyamine that step B obtains, be placed in four-hole boiling flask; Temperature of reaction is risen to 80 DEG C, reaction 2-4h; Temperature of reaction is risen to 90 DEG C, reaction 2-4h; Underpressure distillation, removes unnecessary polyethylene polyamine; Add mono-epoxy compounds after being down to room temperature, maintain temperature of reaction 60 DEG C, reaction 4-6h;
D, add Glacial acetic acid, maintain temperature of reaction 40 DEG C, reaction 4-6h, obtains polyether-type epoxy resin solidifying agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510691984.7A CN105315436A (en) | 2015-10-23 | 2015-10-23 | Polyether type epoxy resin curing agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510691984.7A CN105315436A (en) | 2015-10-23 | 2015-10-23 | Polyether type epoxy resin curing agent and preparation method thereof |
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| CN105315436A true CN105315436A (en) | 2016-02-10 |
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| CN201510691984.7A Pending CN105315436A (en) | 2015-10-23 | 2015-10-23 | Polyether type epoxy resin curing agent and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106397780A (en) * | 2016-09-13 | 2017-02-15 | 安徽大学 | Preparation method of functional epoxy resin curing agent |
| CN106543414A (en) * | 2016-10-12 | 2017-03-29 | 湖北绿色家园精细化工股份有限公司 | A kind of preparation method of novel flexible epoxy resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050300A (en) * | 2007-04-18 | 2007-10-10 | 广州秀珀化工有限公司 | Self-emulsifying type aqueous latex of epoxy hardener, and preparation method |
| CN101759859A (en) * | 2009-12-25 | 2010-06-30 | 巨石集团有限公司 | Production method of epoxy resin emulsion film-forming agent for direct-roving treating compound |
| CN103450448A (en) * | 2012-05-31 | 2013-12-18 | 中国石油化工股份有限公司 | Preparation method of compound aqueous curing agent |
-
2015
- 2015-10-23 CN CN201510691984.7A patent/CN105315436A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050300A (en) * | 2007-04-18 | 2007-10-10 | 广州秀珀化工有限公司 | Self-emulsifying type aqueous latex of epoxy hardener, and preparation method |
| CN101759859A (en) * | 2009-12-25 | 2010-06-30 | 巨石集团有限公司 | Production method of epoxy resin emulsion film-forming agent for direct-roving treating compound |
| CN103450448A (en) * | 2012-05-31 | 2013-12-18 | 中国石油化工股份有限公司 | Preparation method of compound aqueous curing agent |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106397780A (en) * | 2016-09-13 | 2017-02-15 | 安徽大学 | Preparation method of functional epoxy resin curing agent |
| CN106397780B (en) * | 2016-09-13 | 2019-05-21 | 安徽大学 | A kind of preparation method of functional epoxy resin curing agent |
| CN106543414A (en) * | 2016-10-12 | 2017-03-29 | 湖北绿色家园精细化工股份有限公司 | A kind of preparation method of novel flexible epoxy resin |
| CN106543414B (en) * | 2016-10-12 | 2019-08-02 | 湖北绿色家园材料技术股份有限公司 | A kind of preparation method of flexible-epoxy |
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Application publication date: 20160210 |
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