CN101463180B - Aqueous single-component external emulsion epoxy resin emulsion and preparation thereof - Google Patents
Aqueous single-component external emulsion epoxy resin emulsion and preparation thereof Download PDFInfo
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- CN101463180B CN101463180B CN2007100327066A CN200710032706A CN101463180B CN 101463180 B CN101463180 B CN 101463180B CN 2007100327066 A CN2007100327066 A CN 2007100327066A CN 200710032706 A CN200710032706 A CN 200710032706A CN 101463180 B CN101463180 B CN 101463180B
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Abstract
The invention discloses an aqueous one-component external emulsifying epoxide resin latex emulsion and a preparation method thereof. The method comprises: epoxide resin, curing agent, anionic emulsifier, nonionic emulsifier, reactive diluent and solvent are evenly mixed together, and then are stirred at high speed; the mixture is added into the water to be dispersed to obtain the aqueous epoxide resin latex emulsion. The invention adopts emulsifier to emulsify the epoxide resin, so as to lead the hydrophobe epoxide resin to have hydrophilic part, thus being well dispersed in the water.
Description
Technical field
The present invention relates to chemical field, particularly a kind of aqueous single-component external emulsion epoxy resin emulsion and preparation method thereof.
Background technology
Traditional epoxy resin is solvent-borne type and powder-type, has good intensity, wear resistance, chemical resistant properties, erosion resistance etc.But the coating density of powder-type epoxy resin is relatively poor, and difficulty of construction is bigger, need could construct by some specific equipments; Solvent epoxy varnish is a large amount of solvent of meeting volatilization in construction process, contaminate environment, and also some deleterious solvent (such as the triphen class) also can have bigger injury effect to human body.In recent years, about the law and the rules of environmental pollution restriction are put into effect in succession, the system of zero VOC or low VOC has become the research direction of novel material.Aqueous epoxy resins has lot of advantages, as low VOC content, safe in utilization, can wash by water, technology is increasingly mature, compliance with environmental protection requirements etc.; And aqueous epoxy resins can solidify under the environment of room temperature or humidity, and set time and temperature can be adjusted according to construction requirement.At present; Preparation method of water-dilutable epoxide resin has following several kinds: a kind of preparation method makes water-based to solidifying agent; Add epoxy resin, thinner etc. in the waterborne curing agent at the construction field (site), disperseing becomes aqueous epoxy resins, is 200410051180.2 patent like application number; But; Because hydrophilic solidifying agent and the hydrophobic epoxy resin huge difference aspect hydrophilic; Make both on solubility parameters, mismatch, thereby cause being separated after the film forming, cause degradation such as intensity; And, there is not completely crued thinner so also can discharge some behind the epoxy resin cure because system has been used thinner.Another kind of preparation method makes water-based emulsion to epoxy resin earlier, also makes waterborne curing agent to solidifying agent, makes two component systems then.Because epoxy resin is hydrophobic, just must introduce hydrophilic radical so will be distributed to it in the water.Second kind is epoxy resin emulsification, can be divided into outer emulsion process such as US3945964 and internal emulsification method such as US4197389.Outer emulsion process is exactly by means of the emulsifying agent that adds, and liquid or ground solid epoxy are scattered in the water through mechanical stirring, forms stable O/w emulsion system.Outer emulsion process can be divided into direct emulsion process and phase reversion method, still, the emulsion system less stable that direct emulsification obtains, particle is thicker, and is wayward.And technology is complicated, adopts outer emulsification method like US3945964, and needs and solidifying agent could use after mixing.
Summary of the invention
The objective of the invention is to overcome the shortcoming that exists in the prior art, a kind of environmental friendliness, low, the simple aqueous single-component external emulsion epoxy resin emulsion of technology of cost are provided.
Another object of the present invention is to provide a kind of preparation method of above-mentioned aqueous single-component external emulsion epoxy resin emulsion.
The object of the invention is realized through following technical proposals:
A kind of aqueous single-component external emulsion epoxy resin emulsion by weight percentage, comprises following raw material:
Epoxy resin 20~60%
Solidifying agent 1~10%
Nonionic emulsifying agent 1~10%
Anionic emulsifier 1~10%
Reactive thinner 0~10%
Solvent 0~10%
Water 30~70%.
Said epoxy resin can be one or more mixtures in bisphenol A type epoxy resin, phenol aldehyde type epoxy resin, o-cresol formaldehyde type epoxy resin or the polyol shrinkaging glycerin ether type epoxy resin; Preferred bisphenol A type epoxy resin, as: one or more mixtures among E-20, E-44, E-51, EP-828 or the F-51.
Said solidifying agent is a latent curing agent, like Dyhard RU 100 series or imidazoles-metal salt complex etc., and preferred Dyhard RU 100 series.
Said nonionic emulsifying agent can be TX10 (OP series, NP serial) or sorbitol anhydride mono-laurate (trade name is a sapn); The emulsifying agent of preferred OP, NP series.
Said anionic emulsifier can be alkyl-sulphate, AS or alkylphosphonic; Preferred alkyl vitriol or AS.
Said reactive thinner is the low viscosity epoxy resin of monofunctional, like phenyl glycidyl ether or butylglycidyl ether.
Said solvent can be water-soluble solvents such as acetone, butanone, ethanol, Virahol, propyl carbinol, ethylene glycol monomethyl ether or ethylene glycol monobutyl ether.
The preparation method of above-mentioned aqueous single-component external emulsion epoxy resin emulsion; Be under 20~50 ℃; Epoxy resin, solidifying agent, nonionic emulsifying agent, anionic emulsifier, reactive thinner and the solvent of said ratio is even; Under high-speed stirring, add and disperse to obtain aqueous single-component external emulsion epoxy resin emulsion in the entry then.
The present invention compared with prior art has following advantage and effect:
(1) the present invention adopts emulsifying agent that epoxy resin is carried out emulsification, makes hydrophobic epoxy resin have hydrophilic part, thereby can be good at being scattered in the water.
(2) the present invention is distributed to epoxy resin and solidifying agent in the water together; Utilize solidifying agent discord epoxy resin reaction under the normal temperature; The principle of just reacting with epoxy resin behind the elevated temperature obtains the aqueous epoxy resin emulsion of the single component of excellent property, and it can directly use in use; Needn't simplify use technology mixing the back to epoxy resin latex and waterborne curing agent using.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description, but embodiment of the present invention is not limited thereto.
Embodiment 1
With 100gE-51 (E-represents bisphenol A type epoxy resin), the 8g Dyhard RU 100,5gOP-10, the 1g sodium lauryl sulphate adds in the there-necked flask together; Under the oil bath heating, be heated to 50 ℃, mixed 0.5 hour; Under high-speed stirring, slowly add the 170g deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 40% aqueous epoxy resin emulsion.
Embodiment 2
With 1KgE-44, the 73g Dyhard RU 100,60gNP-9, the 10g sodium lauryl sulphate adds in the there-necked flask together; Under oil bath heating, be heated to 30 ℃, mixed 1 hour, wait mix after; Under high-speed stirring, slowly add the 1.4Kg deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 45% epoxy emulsion.
Embodiment 3
With 500gE-20,15g Dyhard RU 100,10g phenyl glycidyl ether, 10g propyl carbinol; 18gOP-9,5g sodium laurylsulfonate add in the there-necked flask together, under the oil bath heating, are heated to 20 ℃; Mixed 1 hour, wait mix after, under high-speed stirring, slowly add the 822g deionized water; After water added fully, restir 0.5 hour filtered, and obtains 40% epoxy emulsion.
Embodiment 4
With 1KgE-44, the 70g Dyhard RU 100, the 40g Arlacel-20, the 15g sodium lauryl sulphate adds in the there-necked flask together; Under the oil bath heating, be heated to 30 ℃, mixed 1 hour, after mixing by the time; Under high-speed stirring, slowly add the 1.12Kg deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 50% epoxy emulsion.
Embodiment 5
With 1KgEP-828, the 80g Dyhard RU 100,65gOP-10, the 12g sodium lauryl sulphate adds in the there-necked flask together; Under the oil bath heating, be heated to 50 ℃, mixed 0.5 hour; Under high-speed stirring, slowly add the 1.735Kg deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 40% aqueous epoxy resin emulsion.
Embodiment 6
With 100gF-51,8g Dyhard RU 100,10g ethylene glycol monobutyl ether, 5gOP-10; The 1g sodium lauryl sulphate adds in the there-necked flask together, under the oil bath heating, is heated to 40 ℃, mixes 0.5 hour; Under high-speed stirring, slowly add the 160g deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 40% aqueous epoxy resin emulsion.
Embodiment 7
With 100gF-51,7g Dyhard RU 100,5g propyl carbinol, 6gNP-30; 1g alkylphosphonic acid carboxylic acid sodium adds in the there-necked flask together, under the oil bath heating, is heated to 50 ℃, mixes 0.5 hour; Under high-speed stirring, slowly add the 170g deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 40% aqueous epoxy resin emulsion.
Claims (5)
1. aqueous single-component external emulsion epoxy resin emulsion, it is characterized in that taking following method to prepare: with 100gE-51, wherein E represents bisphenol A type epoxy resin, the 8g Dyhard RU 100; 5gOP-10, the 1g sodium lauryl sulphate adds in the there-necked flask together, under the oil bath heating, is heated to 50 ℃; Mixed 0.5 hour, and under high-speed stirring, slowly added the 170g deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 40% aqueous epoxy resin emulsion.
2. aqueous single-component external emulsion epoxy resin emulsion is characterized in that taking following method to prepare: with 1KgE-44, and 73g Dyhard RU 100,60gNP-9; The 10g sodium lauryl sulphate adds in the there-necked flask together, under the oil bath heating, is heated to 30 ℃, mixes 1 hour; After mixing, under high-speed stirring, slowly add the 1.4Kg deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 45% epoxy emulsion.
3. aqueous single-component external emulsion epoxy resin emulsion is characterized in that taking following method to prepare: with 500gE-20, and 15g Dyhard RU 100,10g phenyl glycidyl ether, 10g propyl carbinol; 18gOP-9,5g sodium laurylsulfonate add in the there-necked flask together, under the oil bath heating, are heated to 20 ℃; Mixed 1 hour, wait mix after, under high-speed stirring, slowly add the 822g deionized water; After water added fully, restir 0.5 hour filtered, and obtains 40% epoxy emulsion.
4. aqueous single-component external emulsion epoxy resin emulsion is characterized in that taking following method to prepare: with 1KgE-44, and 70g Dyhard RU 100,40g Arlacel-20; The 15g sodium lauryl sulphate adds in the there-necked flask together, under the oil bath heating, is heated to 30 ℃, mixes 1 hour; By the time after mixing, under high-speed stirring, slowly add the 1.12Kg deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 50% epoxy emulsion.
5. aqueous single-component external emulsion epoxy resin emulsion is characterized in that taking following method to prepare: with 1KgEP-828, and 80g Dyhard RU 100,65gOP-10; The 12g sodium lauryl sulphate adds in the there-necked flask together, under the oil bath heating, is heated to 50 ℃, mixes 0.5 hour; Under high-speed stirring, slowly add the 1.735Kg deionized water, after water adds fully; Restir 0.5 hour filters, and obtains 40% aqueous epoxy resin emulsion.
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CN101812218A (en) * | 2010-04-16 | 2010-08-25 | 上海富朗化工科技发展有限公司 | Reactive water-dispersed epoxy resin emulsion and preparation method thereof |
CN102010607B (en) * | 2010-12-02 | 2012-08-01 | 东莞市东物合成材料有限公司 | Thermosetting emulsified epoxy resin modified emulsified asphalt |
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CN104710581A (en) * | 2014-12-31 | 2015-06-17 | 佛山市顺德区巴德富实业有限公司 | Mono-component aqueous epoxy emulsion used for priming paint and preparation method thereof |
CN105001432A (en) * | 2015-07-28 | 2015-10-28 | 何肖凤 | Method for preparing water-borne epoxy resin emulsion |
CN106221506B (en) * | 2016-08-30 | 2017-06-30 | 河北晨阳工贸集团有限公司 | A kind of epoxy emulsion and preparation method thereof |
CN109370153A (en) * | 2018-04-26 | 2019-02-22 | 苏州宇江建材有限公司 | A kind of aqueous epoxy emulsion and preparation method thereof reacted that can mix with oiliness curing agent |
CN110358112B (en) * | 2019-07-16 | 2022-05-13 | 江苏丰彩建材(集团)有限公司 | Preparation method of solid epoxy resin emulsion |
CN111040191A (en) * | 2019-12-25 | 2020-04-21 | 陕西宝塔山油漆股份有限公司 | Environment-friendly water-based epoxy resin emulsion and preparation method thereof |
CN112778879B (en) * | 2021-01-29 | 2022-07-22 | 固德电材系统(苏州)股份有限公司 | Single-component water-based epoxy emulsion and preparation method and application thereof |
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US3945964A (en) * | 1971-03-19 | 1976-03-23 | Garth Winton Hastings | Aqueous epoxy emulsions |
GB2261664A (en) * | 1991-10-22 | 1993-05-26 | Coates Brothers Plc | Coating compositions |
CN1752163A (en) * | 2005-10-20 | 2006-03-29 | 同济大学 | A kind of aqueous epoxide resin paint and preparation method thereof |
DE69928082T2 (en) * | 1999-05-06 | 2006-07-20 | Jsr Corp. | Low dielectric constant composition, insulating material, sealing material, and printed circuit board |
CN1891771A (en) * | 2005-07-05 | 2007-01-10 | 浙江安邦新材料发展有限公司 | Epoxy curing agent emulsion for water-based epoxy coating, and its preparing method |
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2007
- 2007-12-19 CN CN2007100327066A patent/CN101463180B/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3945964A (en) * | 1971-03-19 | 1976-03-23 | Garth Winton Hastings | Aqueous epoxy emulsions |
GB2261664A (en) * | 1991-10-22 | 1993-05-26 | Coates Brothers Plc | Coating compositions |
DE69928082T2 (en) * | 1999-05-06 | 2006-07-20 | Jsr Corp. | Low dielectric constant composition, insulating material, sealing material, and printed circuit board |
CN1891771A (en) * | 2005-07-05 | 2007-01-10 | 浙江安邦新材料发展有限公司 | Epoxy curing agent emulsion for water-based epoxy coating, and its preparing method |
CN1752163A (en) * | 2005-10-20 | 2006-03-29 | 同济大学 | A kind of aqueous epoxide resin paint and preparation method thereof |
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Address after: 510650 Guangdong city of Guangzhou province Tianhe District Xing Branch Road No. 368 Patentee after: Guangzhou Chemistry Co., Ltd. Chinese Academy of Sciences Address before: 510650 Guangdong city of Guangzhou province Tianhe District Xing Branch Road No. 368 Patentee before: Guangzhou Inst. of Chemistry, Chinese Academy of Sciences |
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